Login In
2011 Volume 28 Issue 10
2011, 28(10): 1099-1107
doi: 10.3724/SP.J.1095.2011.00645
Abstract:
Several common methods and principles for the visualization of latent fingerprints were introduced.Among them,the development of chemical-physical and chemical methods,for example,multi-metal deposition,ninhydrin,fluorescence material visualization,etc.were reviewed.
Several common methods and principles for the visualization of latent fingerprints were introduced.Among them,the development of chemical-physical and chemical methods,for example,multi-metal deposition,ninhydrin,fluorescence material visualization,etc.were reviewed.
2011, 28(10): 1108-1113
doi: 10.3724/SP.J.1095.2011.00738
Abstract:
Using different viscosity average relative molecular mass of hydroxyethyl cellulose(HEC) as the emulsifier,microcapsules containing emamectin benzoate were prepared by in-situ polymerization.The factors affecting the surface morphology,the particle size and distribution,the encapsulation efficiency and the drug loading were investigated,and the release properties were determined.The results show that the morphology of the microcapsules made by small relative molecular mass HEC is uniform,dense and the microcapsules have no adhesion phenomenon.With the increase of viscosity average relative molecular mass of HEC,the particle size and the size distribution of microcapsules increase,while the encapsulation efficiency and the drug loading decrease.It is showed that the release performances of the microcapsules which prepared by small relative molecular mass HEC are better.
Using different viscosity average relative molecular mass of hydroxyethyl cellulose(HEC) as the emulsifier,microcapsules containing emamectin benzoate were prepared by in-situ polymerization.The factors affecting the surface morphology,the particle size and distribution,the encapsulation efficiency and the drug loading were investigated,and the release properties were determined.The results show that the morphology of the microcapsules made by small relative molecular mass HEC is uniform,dense and the microcapsules have no adhesion phenomenon.With the increase of viscosity average relative molecular mass of HEC,the particle size and the size distribution of microcapsules increase,while the encapsulation efficiency and the drug loading decrease.It is showed that the release performances of the microcapsules which prepared by small relative molecular mass HEC are better.
2011, 28(10): 1114-1121
doi: 10.3724/SP.J.1095.2011.00699
Abstract:
Starch was firstly acylated by acetic anhydride,fluorescein isothiocyanate(FITC) was then covalently attached onto the starch acetate.And the fluorescein-labeled starch acetate could self-assemble to form uniform nanospheres encapsulated with ibuprofen.The controlled-release properties of obtained ibuprofen-loaded fluorescein-labeled starch nanospheres were investigated in details.The amounts of drugloading and release rate could be tuned by changing the amounts of fluorescein-labeled starch acetate,ibuprofen and volume ratio of acetone to water.The results showed that up to 69.5% of the drug could be encapsulated when the amounts of fluorescein-labeled starch acetate and ibuprofen were 200 mg and 60 mg,and the volumes of water and acetone were 50 mL and 20 mL,respectively.The drug release rate in vitro of these nanospheres was 62.7% at 48 h.Moreover,the release process in vitro of the drug-loaded nanospheres was characterized by scanning electron microscope(SEM) and confocal laser scanning microscope(CLSM).
Starch was firstly acylated by acetic anhydride,fluorescein isothiocyanate(FITC) was then covalently attached onto the starch acetate.And the fluorescein-labeled starch acetate could self-assemble to form uniform nanospheres encapsulated with ibuprofen.The controlled-release properties of obtained ibuprofen-loaded fluorescein-labeled starch nanospheres were investigated in details.The amounts of drugloading and release rate could be tuned by changing the amounts of fluorescein-labeled starch acetate,ibuprofen and volume ratio of acetone to water.The results showed that up to 69.5% of the drug could be encapsulated when the amounts of fluorescein-labeled starch acetate and ibuprofen were 200 mg and 60 mg,and the volumes of water and acetone were 50 mL and 20 mL,respectively.The drug release rate in vitro of these nanospheres was 62.7% at 48 h.Moreover,the release process in vitro of the drug-loaded nanospheres was characterized by scanning electron microscope(SEM) and confocal laser scanning microscope(CLSM).
2011, 28(10): 1122-1129
doi: 10.3724/SP.J.1095.2011.00670
Abstract:
Double water-phase polyacylamide(PAM) emulsion has been synthesized by dispersion polymerization of acrylamide(AM) in ethanol/water(90% volume fraction of ethanol) media with poly(vinyl pyrrolidone)(PVP) as the stabilizer,sodium bisulfite and ammonium persulfate as the initiator(I).Influences of polymerization temperature,mass fraction of initiator,AM and stabilizer on monomer conversion,reaction rate,polymer relative molecular mass and emulsion stability have been investigated.The results showed that as the AM mass fraction increased from 10% to 25%,the initial polymerization rate,final conversion of AM,and polymer relative molecular mass also increased.Among them,the initial polymerization rate was increased by 20 times.However,the use of too high monomer mass fraction could cause gelation because of high viscosity and fast reaction rate.With increasing the stabilizer PVP mass fraction,the initial reaction rate and the final conversion of AM decreased,and it was unsuitable for the double water-phase emulsion stability when the mass fraction of PVP was either too high or too low.Increase of the polymerization temperature resulted in a significant increase of reaction rate and decrease of polymer relative molecular mass from 5.08×105 at 20℃ to 0.39×105 at 70℃.The monomer conversion increased and polymer relative molecular mass decreased from 4.31×105 to 3.73×105 as the initiator mass fraction was increased from 0.05% to 0.15%.The induction period appeared within about 20~25 min and the maximum rate was postponed until 60 min as the initiator mass fraction was 0.05%.A double water-phase PAM emulsion with the particle size distribution of 10~75 μm and average particle size of 21.94 μm was synthesized at 30℃ in 6 h when mass fraction of AM,initiator and PVP was 15%,0.05% and 6%,respectively.The emulsion had poor stability because of its broad particle size distribution and large particle size.The relationship of polymerization rate at AM conversion 50% with the mass concentrations of the initiator,AM and stabilizer is as follows:rp=kρI0.33ρAM0.84ρPVP-2.56.The apparent activation energy of the dispersion polymerization is 40.95 kJ/mol.
Double water-phase polyacylamide(PAM) emulsion has been synthesized by dispersion polymerization of acrylamide(AM) in ethanol/water(90% volume fraction of ethanol) media with poly(vinyl pyrrolidone)(PVP) as the stabilizer,sodium bisulfite and ammonium persulfate as the initiator(I).Influences of polymerization temperature,mass fraction of initiator,AM and stabilizer on monomer conversion,reaction rate,polymer relative molecular mass and emulsion stability have been investigated.The results showed that as the AM mass fraction increased from 10% to 25%,the initial polymerization rate,final conversion of AM,and polymer relative molecular mass also increased.Among them,the initial polymerization rate was increased by 20 times.However,the use of too high monomer mass fraction could cause gelation because of high viscosity and fast reaction rate.With increasing the stabilizer PVP mass fraction,the initial reaction rate and the final conversion of AM decreased,and it was unsuitable for the double water-phase emulsion stability when the mass fraction of PVP was either too high or too low.Increase of the polymerization temperature resulted in a significant increase of reaction rate and decrease of polymer relative molecular mass from 5.08×105 at 20℃ to 0.39×105 at 70℃.The monomer conversion increased and polymer relative molecular mass decreased from 4.31×105 to 3.73×105 as the initiator mass fraction was increased from 0.05% to 0.15%.The induction period appeared within about 20~25 min and the maximum rate was postponed until 60 min as the initiator mass fraction was 0.05%.A double water-phase PAM emulsion with the particle size distribution of 10~75 μm and average particle size of 21.94 μm was synthesized at 30℃ in 6 h when mass fraction of AM,initiator and PVP was 15%,0.05% and 6%,respectively.The emulsion had poor stability because of its broad particle size distribution and large particle size.The relationship of polymerization rate at AM conversion 50% with the mass concentrations of the initiator,AM and stabilizer is as follows:rp=kρI0.33ρAM0.84ρPVP-2.56.The apparent activation energy of the dispersion polymerization is 40.95 kJ/mol.
2011, 28(10): 1130-1134
doi: 10.3724/SP.J.1095.2011.00648
Abstract:
Trimethylol propane triacrylate(TMPTA) and polypropylene(PP) powder without any additives were used to prepare long chain branched polypropylene by in situ heat-induction melt-grafting.The long chain branches of PP with molecular mass over twice the molecular mass between successive entanglements(>2Me) have dramatic effect on the rheological properties.The effect of tetramethylthiuram disulfide(TMTD) on the heat-induction melt-grafting was studied.It was found that the grafting degree of TMPTA decreased but the branching efficiency increased when TMTD was added to the system.According to the result of theoretic calculation,the branching frequency increased from 0.03 to 0.34 when TMTD was employed under the same conditions.
Trimethylol propane triacrylate(TMPTA) and polypropylene(PP) powder without any additives were used to prepare long chain branched polypropylene by in situ heat-induction melt-grafting.The long chain branches of PP with molecular mass over twice the molecular mass between successive entanglements(>2Me) have dramatic effect on the rheological properties.The effect of tetramethylthiuram disulfide(TMTD) on the heat-induction melt-grafting was studied.It was found that the grafting degree of TMPTA decreased but the branching efficiency increased when TMTD was added to the system.According to the result of theoretic calculation,the branching frequency increased from 0.03 to 0.34 when TMTD was employed under the same conditions.
2011, 28(10): 1135-1142
doi: 10.3724/SP.J.1095.2011.00650
Abstract:
Acrylic/polyurethane(PUA) hybrid emulsion has been prepared by water-borne polyurethane(WPU) modified with acrylic resin.A method for adding different mass fraction of acrylic(AC) into polyurethane(PU) polymers is proposed and verified through designed experiments.With increasing the polyacrylate(PA) mass fraction in the copolymer,the appearance of the emulsion changes from transparent to opacity,in the meantime,the particle size is increased.The TEM result reveals that PUA latex particles present clear core-shell structure and regular shape,and the size distribution is within the range of 60~120 nm.The results of FTIR indicate that the hydrogen bonding effect of PU hard segment first increased and then decreased,while the ordering of hard segment decreased with increasing the AC mass fraction.Compatibility and degree of mixing were developed under 75% AC added in copolymers.With increasing PA mass fraction,one glass transition temperature existed in the copolymers before the content of AC arrived 75%.Thermogravimetric analysis(TGA) shows that the temperatures for the maximal thermal mass-loss rate rose from 363℃ to 412℃,and water absorption for samples decreased from 11.3% to 5.7% with the increase of AC fraction.Additionally,the elasticity modulus of PUA was raised from 16.4 to 47.6 MPa,while the tensile strength was increased from 9.0 to 23.7 MPa,and the elongation at break changed from 365% to 408%.Furthermore,the composite latex viscosity is decresed,and the drying time is shortened,while glue film adhesion force becomes better.
Acrylic/polyurethane(PUA) hybrid emulsion has been prepared by water-borne polyurethane(WPU) modified with acrylic resin.A method for adding different mass fraction of acrylic(AC) into polyurethane(PU) polymers is proposed and verified through designed experiments.With increasing the polyacrylate(PA) mass fraction in the copolymer,the appearance of the emulsion changes from transparent to opacity,in the meantime,the particle size is increased.The TEM result reveals that PUA latex particles present clear core-shell structure and regular shape,and the size distribution is within the range of 60~120 nm.The results of FTIR indicate that the hydrogen bonding effect of PU hard segment first increased and then decreased,while the ordering of hard segment decreased with increasing the AC mass fraction.Compatibility and degree of mixing were developed under 75% AC added in copolymers.With increasing PA mass fraction,one glass transition temperature existed in the copolymers before the content of AC arrived 75%.Thermogravimetric analysis(TGA) shows that the temperatures for the maximal thermal mass-loss rate rose from 363℃ to 412℃,and water absorption for samples decreased from 11.3% to 5.7% with the increase of AC fraction.Additionally,the elasticity modulus of PUA was raised from 16.4 to 47.6 MPa,while the tensile strength was increased from 9.0 to 23.7 MPa,and the elongation at break changed from 365% to 408%.Furthermore,the composite latex viscosity is decresed,and the drying time is shortened,while glue film adhesion force becomes better.
2011, 28(10): 1143-1147
doi: 10.3724/SP.J.1095.2011.00628
Abstract:
Controlled/living polymerization kinetics of vinyl acetate(VAc) was studied.Poly(vinyl acetate)(PVAc) with predetermined molecular mass and relatively low polydispersity was successfully synthesized from vinyl acetate(VAc) by a degenerative transfer radical polymerization with the presence of iodine(0.57%~0.86% mass fraction of the system) using 2,2'-azobis(isobutyronitrile)(AIBN) as the initiator.The effects of iodine concentration on reaction speed and relative molecular mass and relatively polydispersity were investigated.The results indicated that the increasing speed of molecular mass was successfully controlled and relatively polydispersity was narrowed with increasing iodine concentration.The polymerization was monitored by an on-line 1H NMR spectroscopy to investigate the evolution of several compounds in the reaction medium,especially the adduct between primary radicals and iodine(A-I,where A stands for the radical fragment from the initiator),and the monoadduct A-Mn-I(where M stands for the monomer unit).The structure of the poly(vinyl acetate) iodo-terminated chain end groups by this method was proved using 1H NMR spectrum.Molecular masses increase linearly with conversion and molecular polydispersities decrease gradually with improving monomer conversion of vinyl acetate,and polymers with relatively narrow molecular polydispersities(Mw/Mn ≤ 1.41) are obtained when the monomer conversion of vinyl acetate reaches up to 80%,indicating that the process of degenerative transfer polymerization efficiently controls the number-average molecular mass and molecular polydispersities in the presence of molecular iodine(I2),therefore the process is a controlled/living radical polymerization.
Controlled/living polymerization kinetics of vinyl acetate(VAc) was studied.Poly(vinyl acetate)(PVAc) with predetermined molecular mass and relatively low polydispersity was successfully synthesized from vinyl acetate(VAc) by a degenerative transfer radical polymerization with the presence of iodine(0.57%~0.86% mass fraction of the system) using 2,2'-azobis(isobutyronitrile)(AIBN) as the initiator.The effects of iodine concentration on reaction speed and relative molecular mass and relatively polydispersity were investigated.The results indicated that the increasing speed of molecular mass was successfully controlled and relatively polydispersity was narrowed with increasing iodine concentration.The polymerization was monitored by an on-line 1H NMR spectroscopy to investigate the evolution of several compounds in the reaction medium,especially the adduct between primary radicals and iodine(A-I,where A stands for the radical fragment from the initiator),and the monoadduct A-Mn-I(where M stands for the monomer unit).The structure of the poly(vinyl acetate) iodo-terminated chain end groups by this method was proved using 1H NMR spectrum.Molecular masses increase linearly with conversion and molecular polydispersities decrease gradually with improving monomer conversion of vinyl acetate,and polymers with relatively narrow molecular polydispersities(Mw/Mn ≤ 1.41) are obtained when the monomer conversion of vinyl acetate reaches up to 80%,indicating that the process of degenerative transfer polymerization efficiently controls the number-average molecular mass and molecular polydispersities in the presence of molecular iodine(I2),therefore the process is a controlled/living radical polymerization.
2011, 28(10): 1148-1154
doi: 10.3724/SP.J.1095.2011.00620
Abstract:
A single electron transfer living radical polymerization(SET-LRP) is able to rapidly achieve high molecular mass,with excellent control of molecular mass distribution,represents a robust and versatile method for the rapid synthesis of macromolecules with defined architecture.The SET-LRP of acryl amide(AM) was investigated at 40℃ in 1-butyl,3-methyl tetrafluoroborate([Bmim]BF4) ionic liquid,using Cu0 power/tris(2-dimethylamin ethyl) amine(Me6-TREN) as catalyst,2,2-dibromomethyl-1,3-dibromopropane(PEBr4) as initiator.The polymerization showed some "living" features:the conversion and ln([M]0/[M]) increased linearly with time as well as the number-average molecular mass increased linearly with conversion.The star polyacrylamide(sPAM) prepared via SET-LRP was characterized by GPC and 1H NMR to identify its polymerization mechanism,and the results showed that the polymer had the perfect functional chain ends and relatively low molecular mass distribution Mw/Mn≈1.26(MnGPC=14.1×103,conversion rate is 43.4%),indicating a controlled polymerization.The effects of water,catalyst and initiator on polymerization were studied,and the dynamic experiments were carried out.A small amount of water added could accerlerate the polymerization,the apparent rate constants of propagation(kpapp) were 0.04248 h-1 and 0.14869 h-1 for adding free water and 0.5 mL H2O respectively;the control of polymerization could be improved with the presence of catalyst and increasing the concentration of initiator.The polymerization rate of SET-LRP increased with the amount of catalyst and initiator.In addition,Mn increased with the amount of catalyst or decreasing the amount of initiator and was closed to the theoretical molecular mass.The molecular mass distribution showed a decreasing trend,the minimum was about 1.26.The[Bmim]BF4 ionic liquid was a good solvent to PEBr4 and acryl amide,and the polymers were easily separated from the catalyst.
A single electron transfer living radical polymerization(SET-LRP) is able to rapidly achieve high molecular mass,with excellent control of molecular mass distribution,represents a robust and versatile method for the rapid synthesis of macromolecules with defined architecture.The SET-LRP of acryl amide(AM) was investigated at 40℃ in 1-butyl,3-methyl tetrafluoroborate([Bmim]BF4) ionic liquid,using Cu0 power/tris(2-dimethylamin ethyl) amine(Me6-TREN) as catalyst,2,2-dibromomethyl-1,3-dibromopropane(PEBr4) as initiator.The polymerization showed some "living" features:the conversion and ln([M]0/[M]) increased linearly with time as well as the number-average molecular mass increased linearly with conversion.The star polyacrylamide(sPAM) prepared via SET-LRP was characterized by GPC and 1H NMR to identify its polymerization mechanism,and the results showed that the polymer had the perfect functional chain ends and relatively low molecular mass distribution Mw/Mn≈1.26(MnGPC=14.1×103,conversion rate is 43.4%),indicating a controlled polymerization.The effects of water,catalyst and initiator on polymerization were studied,and the dynamic experiments were carried out.A small amount of water added could accerlerate the polymerization,the apparent rate constants of propagation(kpapp) were 0.04248 h-1 and 0.14869 h-1 for adding free water and 0.5 mL H2O respectively;the control of polymerization could be improved with the presence of catalyst and increasing the concentration of initiator.The polymerization rate of SET-LRP increased with the amount of catalyst and initiator.In addition,Mn increased with the amount of catalyst or decreasing the amount of initiator and was closed to the theoretical molecular mass.The molecular mass distribution showed a decreasing trend,the minimum was about 1.26.The[Bmim]BF4 ionic liquid was a good solvent to PEBr4 and acryl amide,and the polymers were easily separated from the catalyst.
2011, 28(10): 1155-1160
doi: 10.3724/SP.J.1095.2011.00659
Abstract:
The saturated red polymer electrophosphorescent devices have been fabricated.With the device structures of ITO/PEDOT:PSS/PVK/PFO+30% PBD:TDPPPt/Ca/Al(ITO:indium tin oxide,PEDOT:poly(3,4-ethylenedioxythiophene),PSS:poly(styrenesulfonate),PVK:poly N-vinyl carbazole),based on short lifetime meso-tetrakis(4-n-decanoyl-phenyl) porphyrin platinum(Ⅱ) complex(TDPPPt) and poly(2,7-9,9-dioctylfluorene)(PFO) in which 30% 2-(bi-phenyl-4-yl)-5-(4-tert-butylphenyl)-1,3,4-oxadiazole(PBD) was doped.The saturated red emission is obtained when doping concentration of TDPPPt is 3%~10%.The CIE(Commission Internationale de L'Eclairage) coordinates of the device is about at(0.66,0.28) and unchangeable when driven voltage increases from 7 V to 14 V.The maximum luminance and luminance efficiency(ηl) is 1 390 cd/m2 at 18 V and 1.34 cd/A at 18×10-3 A/cm2,respectively.Furthermore,the devices show excellent stability under high driven current density.ηl only drops to 88% and 73% of maximum efficiency at 100×10-3 A/cm2,and 150×10-3 A/cm2,respectively.We tentatively attribute excellent devices stability under high driven current density to the short radiative lifetime that avoids triplet-triple annihilation.
The saturated red polymer electrophosphorescent devices have been fabricated.With the device structures of ITO/PEDOT:PSS/PVK/PFO+30% PBD:TDPPPt/Ca/Al(ITO:indium tin oxide,PEDOT:poly(3,4-ethylenedioxythiophene),PSS:poly(styrenesulfonate),PVK:poly N-vinyl carbazole),based on short lifetime meso-tetrakis(4-n-decanoyl-phenyl) porphyrin platinum(Ⅱ) complex(TDPPPt) and poly(2,7-9,9-dioctylfluorene)(PFO) in which 30% 2-(bi-phenyl-4-yl)-5-(4-tert-butylphenyl)-1,3,4-oxadiazole(PBD) was doped.The saturated red emission is obtained when doping concentration of TDPPPt is 3%~10%.The CIE(Commission Internationale de L'Eclairage) coordinates of the device is about at(0.66,0.28) and unchangeable when driven voltage increases from 7 V to 14 V.The maximum luminance and luminance efficiency(ηl) is 1 390 cd/m2 at 18 V and 1.34 cd/A at 18×10-3 A/cm2,respectively.Furthermore,the devices show excellent stability under high driven current density.ηl only drops to 88% and 73% of maximum efficiency at 100×10-3 A/cm2,and 150×10-3 A/cm2,respectively.We tentatively attribute excellent devices stability under high driven current density to the short radiative lifetime that avoids triplet-triple annihilation.
2011, 28(10): 1161-1166
doi: 10.3724/SP.J.1095.2011.00609
Abstract:
Ferrocene-terminated phenylethynythiol derivatives 1 and 2 were prepared from S-acetyl-4-iodothiophenol(6) or 4-iodophenyl methyl sulfide(7) and ethynylferrocene via cross-coupling reactions.Compounds 6 and 7 were prepared in a good yield with Zn/Me2SiCl2/DMA(N,N-dimethylacet amide) reduction system at room temperature instead of traditional low temperature metal lithium system(-78℃).The spectral characteristics,electrochemical properties and self-assembly behaviors of the target compounds on Au modified glassy carbon electrodes(Au/GCE) were investigated.Compound 1 film coated Au/GCE has high electrocatalytic activity toward the oxidation of rutin and has potential applications as biosensor and electrochemical sensor.
Ferrocene-terminated phenylethynythiol derivatives 1 and 2 were prepared from S-acetyl-4-iodothiophenol(6) or 4-iodophenyl methyl sulfide(7) and ethynylferrocene via cross-coupling reactions.Compounds 6 and 7 were prepared in a good yield with Zn/Me2SiCl2/DMA(N,N-dimethylacet amide) reduction system at room temperature instead of traditional low temperature metal lithium system(-78℃).The spectral characteristics,electrochemical properties and self-assembly behaviors of the target compounds on Au modified glassy carbon electrodes(Au/GCE) were investigated.Compound 1 film coated Au/GCE has high electrocatalytic activity toward the oxidation of rutin and has potential applications as biosensor and electrochemical sensor.
2011, 28(10): 1167-1172
doi: 10.3724/SP.J.1095.2011.00618
Abstract:
Four coordination compounds of transition metal with 3,5-diiodo-salicylalidehyde and salicyhydrazide Schiff base have been synthesized in pyridine and DMF solvents.These ligand and complexes were characterized by UV and IR spectra,TG-DTG,elemental analysis,and molar conductance analysis.The interactions of the complexes with DNA were investigated by UV and fluorescence spectroscopies,which show that the binding mode of the complexes with ct-DNA was intercalation.In addition,the biological activity test reveals that the complexes have potentially catalytic and antibacterial activity towards superoxide anion radical O2-· and Micrococcus luteus.
Four coordination compounds of transition metal with 3,5-diiodo-salicylalidehyde and salicyhydrazide Schiff base have been synthesized in pyridine and DMF solvents.These ligand and complexes were characterized by UV and IR spectra,TG-DTG,elemental analysis,and molar conductance analysis.The interactions of the complexes with DNA were investigated by UV and fluorescence spectroscopies,which show that the binding mode of the complexes with ct-DNA was intercalation.In addition,the biological activity test reveals that the complexes have potentially catalytic and antibacterial activity towards superoxide anion radical O2-· and Micrococcus luteus.
2011, 28(10): 1173-1178
doi: 10.3724/SP.J.1095.2011.00633
Abstract:
A series of novel N-[2-(4,6-dimethoxypyrimidin-2-yloxy) benzylidene]-2-aryloxyacetohydrazides 3 was synthesized by the condensation reactions of 2-(4,6-dimethoxypyrimidin-2-yloxy) benzaldehyde 1 with various 2-aryloxyacetohydrazides 2.Their structures were characterized by IR,1H NMR,EI-MS,ESI-MS and elemental analysis.The results of bioassay(in vivo) indicated that most of the title compounds 3 possessed good herbicidal activities against Amaranthus retroflexus in both pre-emergence and post-emergence treatments at the dose of 1.5 kg/hm2.
A series of novel N-[2-(4,6-dimethoxypyrimidin-2-yloxy) benzylidene]-2-aryloxyacetohydrazides 3 was synthesized by the condensation reactions of 2-(4,6-dimethoxypyrimidin-2-yloxy) benzaldehyde 1 with various 2-aryloxyacetohydrazides 2.Their structures were characterized by IR,1H NMR,EI-MS,ESI-MS and elemental analysis.The results of bioassay(in vivo) indicated that most of the title compounds 3 possessed good herbicidal activities against Amaranthus retroflexus in both pre-emergence and post-emergence treatments at the dose of 1.5 kg/hm2.
2011, 28(10): 1179-1183
doi: 10.3724/SP.J.1095.2011.00647
Abstract:
This paper discussed the Ullmann reaction of aryl halides with nitrogen heterocycles catalyzed by copper(Ⅰ) iodide/ethylenediamine.The results showed that reaction was preferred for nitrogen heterocycles with lower pKa values.In addition,the reactions were also favorable for the electron-rich aryl halides with p-π conjugations,however,they became difficult for other electron-rich aryl halides.
This paper discussed the Ullmann reaction of aryl halides with nitrogen heterocycles catalyzed by copper(Ⅰ) iodide/ethylenediamine.The results showed that reaction was preferred for nitrogen heterocycles with lower pKa values.In addition,the reactions were also favorable for the electron-rich aryl halides with p-π conjugations,however,they became difficult for other electron-rich aryl halides.
2011, 28(10): 1184-1188
doi: 10.3724/SP.J.1095.2011.00677
Abstract:
Four different sodium sulfosuccinates were synthesized using 1-dodecanol,1-tetradecanol,1-hexadecanol,1-octadecanol,maleic anhydride and ethylene glycol as starting materials.The structures of the target compounds were identified by IR and 1H NMR.The results of surface tensions,foaming abilities and emulsifiability measuring show that every compound has lower critical micelle concentration(cmc),stronger emulsifying and better foaming ability.In addition,the structures and the performance relations of the four compounds were discussed.
Four different sodium sulfosuccinates were synthesized using 1-dodecanol,1-tetradecanol,1-hexadecanol,1-octadecanol,maleic anhydride and ethylene glycol as starting materials.The structures of the target compounds were identified by IR and 1H NMR.The results of surface tensions,foaming abilities and emulsifiability measuring show that every compound has lower critical micelle concentration(cmc),stronger emulsifying and better foaming ability.In addition,the structures and the performance relations of the four compounds were discussed.
2011, 28(10): 1189-1194
doi: 10.3724/SP.J.1095.2011.00642
Abstract:
A facile and efficient synthesis route for the preparation of high entropy Nd-Fe-Co-Ni-Mn alloy films was reported.Here the films with nanostructures were successfully synthesized by electrodeposition at room temperature.By changing the electrodeposition parameters,such as the deposition potential and deposition time,the styles of the nanostructures and surface morphologies of the deposits can be well controlled.The SEM images show that the surfaces of the films,prepared at-2.2 V on Ti substrates for 5 min,are composed of great deal of close-grained and homogeneous nanoparticles with size about 200 nm.The film will become more compact with a longer deposition time.When the deposition potential was shifted negatively without changing other conditions,nanosheets can be successfully prepared.The EDS indicates that the five elements are co-deposited.We conclude a typical induced codeposition of Nd and the transition elements does occur in DMSO.The result of XRD suggested that the film was amorphous.The as-deposited alloys show soft magnetic properties.
A facile and efficient synthesis route for the preparation of high entropy Nd-Fe-Co-Ni-Mn alloy films was reported.Here the films with nanostructures were successfully synthesized by electrodeposition at room temperature.By changing the electrodeposition parameters,such as the deposition potential and deposition time,the styles of the nanostructures and surface morphologies of the deposits can be well controlled.The SEM images show that the surfaces of the films,prepared at-2.2 V on Ti substrates for 5 min,are composed of great deal of close-grained and homogeneous nanoparticles with size about 200 nm.The film will become more compact with a longer deposition time.When the deposition potential was shifted negatively without changing other conditions,nanosheets can be successfully prepared.The EDS indicates that the five elements are co-deposited.We conclude a typical induced codeposition of Nd and the transition elements does occur in DMSO.The result of XRD suggested that the film was amorphous.The as-deposited alloys show soft magnetic properties.
2011, 28(10): 1195-1201
doi: 10.3724/SP.J.1095.2011.00683
Abstract:
Spherical silica nanoparticles with average particle size of 10 nm were synthesized using sodium silicate extracted from oil shale ash as silica source.The results showed that the addition of poly(ethylene glycol)(PEG) could effectively prevent the aggregation of silica nanoparticles and tune the particle size,the optimal PEG concentration was found to be 3.0%.Ultrasonication is a key factor to the formation of small,uniform nanoparticles and an optimized hydrolysis-condensation period for ultrasonication is 0.5 h.The azeotropic distillation evidently suppresses agglomeration and a possible mechanism of azeotropic distillation was also proposed.
Spherical silica nanoparticles with average particle size of 10 nm were synthesized using sodium silicate extracted from oil shale ash as silica source.The results showed that the addition of poly(ethylene glycol)(PEG) could effectively prevent the aggregation of silica nanoparticles and tune the particle size,the optimal PEG concentration was found to be 3.0%.Ultrasonication is a key factor to the formation of small,uniform nanoparticles and an optimized hydrolysis-condensation period for ultrasonication is 0.5 h.The azeotropic distillation evidently suppresses agglomeration and a possible mechanism of azeotropic distillation was also proposed.
2011, 28(10): 1202-1207
doi: 10.3724/SP.J.1095.2011.00658
Abstract:
1-Ethylbenzimidazolium(eBim),1-ethyl-3-butyl-benzimi dazoliumbromine(C4eBimBr) intermediates,and 1-ethyl-3-butyl-benzimidazoliumhexafluorophosphate(C4eBimPF6) ionic liquid were synthesized.The structures of the intermediates and the ionic liquid were analyzed with IR and nuclear magnetic resonance spectroscopies.An analytical method for the determination of dioctyl phthalate(DOP) and dinonyl phthalate(DIP) in water using ionic liquid-based microextraction coupled with high performance liquid chromatography was developed.The influence of the extraction parameters including the extraction temperature,extraction time,and amount of ionic liquid was investigated.In the range from 1.0~10 μg/L,the relationship between the peak height and concentration of DOP and DNP was linear,and the correlative coefficients were 0.9847 and 0.9872 respectively.The limits of detection of the DOP and DNP were 0.018 and 0.052 μg/L,recoveries of DOP and DNP were 94.3%~102% and 93.5%~103%,respectively.
1-Ethylbenzimidazolium(eBim),1-ethyl-3-butyl-benzimi dazoliumbromine(C4eBimBr) intermediates,and 1-ethyl-3-butyl-benzimidazoliumhexafluorophosphate(C4eBimPF6) ionic liquid were synthesized.The structures of the intermediates and the ionic liquid were analyzed with IR and nuclear magnetic resonance spectroscopies.An analytical method for the determination of dioctyl phthalate(DOP) and dinonyl phthalate(DIP) in water using ionic liquid-based microextraction coupled with high performance liquid chromatography was developed.The influence of the extraction parameters including the extraction temperature,extraction time,and amount of ionic liquid was investigated.In the range from 1.0~10 μg/L,the relationship between the peak height and concentration of DOP and DNP was linear,and the correlative coefficients were 0.9847 and 0.9872 respectively.The limits of detection of the DOP and DNP were 0.018 and 0.052 μg/L,recoveries of DOP and DNP were 94.3%~102% and 93.5%~103%,respectively.
2011, 28(10): 1208-1212
doi: 10.3724/SP.J.1095.2011.00639
Abstract:
A new method using microcrystalline anthracene as an adsorbent to separate and preconcentrate trace copper in environmental water samples has been developed.Effects of different parameters,such as the acidity,types of salt,amounts of 1-(2-pyridylazo)-2-naphthol(PAN) and anthracene,preconcentration time,etc.on the enrichment yield of Cu(Ⅱ) have been investigated.The results indicate that at pH=3.00,a red chelate complex generated by the reaction between Cu(Ⅱ) and PAN can be quantitatively adsorbed on the surface of microcrystalline anthracene,whereas Pb(Ⅱ),Mn(Ⅱ),Co(Ⅱ),Ni(Ⅱ),Cd(Ⅱ),Zn(Ⅱ),Fe(Ⅲ),Al(Ⅲ) etc.completely remain in the solution.Therefore,the aim of separation and preconcentration of trace copper could be achieved.The possible reaction mechanism of the enrichment of copper is discussed in detail in this paper.The recovery is in the range of 91.0%~104.0% with the enrichment factor of 200.The limit of detection after preconcentration is 0.026 μg/L.The proposed method could be directly applied to the determination of trace copper in different environmental water samples of large volume(1 L) with satisfactory results.
A new method using microcrystalline anthracene as an adsorbent to separate and preconcentrate trace copper in environmental water samples has been developed.Effects of different parameters,such as the acidity,types of salt,amounts of 1-(2-pyridylazo)-2-naphthol(PAN) and anthracene,preconcentration time,etc.on the enrichment yield of Cu(Ⅱ) have been investigated.The results indicate that at pH=3.00,a red chelate complex generated by the reaction between Cu(Ⅱ) and PAN can be quantitatively adsorbed on the surface of microcrystalline anthracene,whereas Pb(Ⅱ),Mn(Ⅱ),Co(Ⅱ),Ni(Ⅱ),Cd(Ⅱ),Zn(Ⅱ),Fe(Ⅲ),Al(Ⅲ) etc.completely remain in the solution.Therefore,the aim of separation and preconcentration of trace copper could be achieved.The possible reaction mechanism of the enrichment of copper is discussed in detail in this paper.The recovery is in the range of 91.0%~104.0% with the enrichment factor of 200.The limit of detection after preconcentration is 0.026 μg/L.The proposed method could be directly applied to the determination of trace copper in different environmental water samples of large volume(1 L) with satisfactory results.
2011, 28(10): 1213-1217
doi: 10.3724/SP.J.1095.2011.00624
Abstract:
Copper colloids were synthesized in ethylene glycol by using ascorbic acid(VC) as the reducing agent and polyvinyl pyrrolidone(PVP) as the dispersant.The as-prepared copper colloids were characterized by XRD,UV-Vis and resonance light scattering(RLS).Face-centered cubic Cu(0) particles were formed,which displayed resonance light scattering(RLS) spectra with a typical plasma resonance absorption within the range of 592~602 nm and the maximum scattering wavelength at 468 nm.The RLS results show that the favorable reaction conditions are in the addition order of VC,CuSO4 and PVP under n(VC)/n(Cu2+)=15,n(PVP-K30)/n(Cu2+)=1.4,temperature=60℃,and incubating for 1 h.The obtained copper colloids are stable for 24 h.Under such reaction conditions,the scattering intensity(ΔIRLS) is proportional to Cu2+ content in the range of 5.12~12.8 mg/L with the detection limit of 0.63 μg/L(3σ),and the regression equation is ΔI=7420.2ρ-631.8(r=0.9962).When the concentration of Cu2+ solution is 10 mg/L,the colloidal system is stable for 24 h.Foreign substances such as 0.64 mg/L MnSO4,CdSO4 and ZnSO4,1.28 mg/L of KI,64 mg/L of Na2CO3 and Ca(OH)2,960 mg/L CH3CH2OH,640 mg/L CH3OH and 320 mg/L CH3CH2CH2OH had no interference.Therefore,a simple method to detect the Cu2+ in ethylene glycol is established using the RLS spectra.
Copper colloids were synthesized in ethylene glycol by using ascorbic acid(VC) as the reducing agent and polyvinyl pyrrolidone(PVP) as the dispersant.The as-prepared copper colloids were characterized by XRD,UV-Vis and resonance light scattering(RLS).Face-centered cubic Cu(0) particles were formed,which displayed resonance light scattering(RLS) spectra with a typical plasma resonance absorption within the range of 592~602 nm and the maximum scattering wavelength at 468 nm.The RLS results show that the favorable reaction conditions are in the addition order of VC,CuSO4 and PVP under n(VC)/n(Cu2+)=15,n(PVP-K30)/n(Cu2+)=1.4,temperature=60℃,and incubating for 1 h.The obtained copper colloids are stable for 24 h.Under such reaction conditions,the scattering intensity(ΔIRLS) is proportional to Cu2+ content in the range of 5.12~12.8 mg/L with the detection limit of 0.63 μg/L(3σ),and the regression equation is ΔI=7420.2ρ-631.8(r=0.9962).When the concentration of Cu2+ solution is 10 mg/L,the colloidal system is stable for 24 h.Foreign substances such as 0.64 mg/L MnSO4,CdSO4 and ZnSO4,1.28 mg/L of KI,64 mg/L of Na2CO3 and Ca(OH)2,960 mg/L CH3CH2OH,640 mg/L CH3OH and 320 mg/L CH3CH2CH2OH had no interference.Therefore,a simple method to detect the Cu2+ in ethylene glycol is established using the RLS spectra.
2011, 28(10): 1218-1220
doi: 10.3724/SP.J.1095.2011.00679
Abstract:
The extraction of lanthanum to a W/O microemulsion by the sodium oleate(NaOL)/pentanol/heptane/NaCl microemulsion system was studied.The influence of extraction time,aqueous-microemulsion ratio,concentration of NaOL,concentration of cosurfactant,pH and salting-out agent on the extraction rate was investigated.The microemulsion system showed strong extractability and stability without extractant.The extraction rate(E%) can be more than 99.5% when the mass fraction of NaOL and pentanol are 6% and 32%,respectively,R=7 and pH 3.5~7.
The extraction of lanthanum to a W/O microemulsion by the sodium oleate(NaOL)/pentanol/heptane/NaCl microemulsion system was studied.The influence of extraction time,aqueous-microemulsion ratio,concentration of NaOL,concentration of cosurfactant,pH and salting-out agent on the extraction rate was investigated.The microemulsion system showed strong extractability and stability without extractant.The extraction rate(E%) can be more than 99.5% when the mass fraction of NaOL and pentanol are 6% and 32%,respectively,R=7 and pH 3.5~7.
