Login In
2011 Volume 28 Issue 1
2011, 28(1): 1-9
doi: 10.3724/SP.J.1095.2011.00205
Abstract:
We present a brief review of recent progress in materials chemistry based on graphene, including the preparation and surface modification of graphene and graphene-based composites. The composites consisted of graphene and polymers, inorganic particles and other carbonaceous materials are described principally. In addition, the prospective applications of these graphene-based materials have also been briefly introduced.
We present a brief review of recent progress in materials chemistry based on graphene, including the preparation and surface modification of graphene and graphene-based composites. The composites consisted of graphene and polymers, inorganic particles and other carbonaceous materials are described principally. In addition, the prospective applications of these graphene-based materials have also been briefly introduced.
2011, 28(1): 10-15
doi: 10.3724/SP.J.1095.2011.00106
Abstract:
5-Butoxymethylenyl-2-norbornene (NBE-CH2OC4H9) was synthesized. Polynorbornenes with functional groups were obtained by homo and copolymerizations of norbornene derivatives catalyzed by bis(β-ketonaphthylamino) Ni(Ⅱ)/B(C6F5)3 system. Influences on polymerizations by changing polymerization time and copolymerization monomer feed ratios was examined. The catalytic bis(β-ketonaphthylamino) Ni(Ⅱ)/B(C6F5)3 system exhibited higher catalysis activity. The obtained polymers were characterized by1H NMR, FTIR and TGA. Results indicated that the incorporation rate could reach 22.1%~76.9% ether units at a molar fraction of 10%~90% of the NBE-CH2 OC4 H9 in the monomer feed ratios; the polymerizations are confirmed to be vinyl-addition mode. The polymer has a good thermal stability(Td >360℃) and is soluble in many common solvents, such as THF and CHCl3.
5-Butoxymethylenyl-2-norbornene (NBE-CH2OC4H9) was synthesized. Polynorbornenes with functional groups were obtained by homo and copolymerizations of norbornene derivatives catalyzed by bis(β-ketonaphthylamino) Ni(Ⅱ)/B(C6F5)3 system. Influences on polymerizations by changing polymerization time and copolymerization monomer feed ratios was examined. The catalytic bis(β-ketonaphthylamino) Ni(Ⅱ)/B(C6F5)3 system exhibited higher catalysis activity. The obtained polymers were characterized by1H NMR, FTIR and TGA. Results indicated that the incorporation rate could reach 22.1%~76.9% ether units at a molar fraction of 10%~90% of the NBE-CH2 OC4 H9 in the monomer feed ratios; the polymerizations are confirmed to be vinyl-addition mode. The polymer has a good thermal stability(Td >360℃) and is soluble in many common solvents, such as THF and CHCl3.
2011, 28(1): 16-21
doi: 10.3724/SP.J.1095.2011.00226
Abstract:
The diffusion of water into polycarbonate film was investigated by attenuated-total-reflection Fourier transform infrared (ATR-FTIR) spectroscopy. Via band deconvolution in the O-H bending region, three components were identified, which were located at 1669, 1648 and 1623 cm-1, respectively, whereas in the O-H stretching region, three bands at 3562, 3423 and 3246 cm-1, respectively were isolated. These results indicate the presence of three states of water molecules in the polycarbonate matrix:strong, moderate, and weak hydrogen-bonded water. Two dimensional correlation analysis of the IR data further confirmed the presence of the three states, and revealed the sequence of the formation of the three types of hydrogen bonding. Based on these experimental results, we concluded that when water diffuses into polycarbonate matrix, it first forms moderate hydrogen bond with the carbonyl group(i. e. the water bound to the carbonyl), followed by the formation of strong hydrogen bonds due to a water molecule bridging a carbonyl and another carbonyl or water molecule, and weak hydrogen bond between water molecules in microvoids.
The diffusion of water into polycarbonate film was investigated by attenuated-total-reflection Fourier transform infrared (ATR-FTIR) spectroscopy. Via band deconvolution in the O-H bending region, three components were identified, which were located at 1669, 1648 and 1623 cm-1, respectively, whereas in the O-H stretching region, three bands at 3562, 3423 and 3246 cm-1, respectively were isolated. These results indicate the presence of three states of water molecules in the polycarbonate matrix:strong, moderate, and weak hydrogen-bonded water. Two dimensional correlation analysis of the IR data further confirmed the presence of the three states, and revealed the sequence of the formation of the three types of hydrogen bonding. Based on these experimental results, we concluded that when water diffuses into polycarbonate matrix, it first forms moderate hydrogen bond with the carbonyl group(i. e. the water bound to the carbonyl), followed by the formation of strong hydrogen bonds due to a water molecule bridging a carbonyl and another carbonyl or water molecule, and weak hydrogen bond between water molecules in microvoids.
2011, 28(1): 22-26
doi: 10.3724/SP.J.1095.2011.00138
Abstract:
Polyaniline(PAN) was in-situ formed around calcium carbonate(CaCO3) microparticles previously stabilized with polyelectrolyte layers (PEs), generating PAN/(PEs)6/CaCO3 hybrid microparticles. The effects of PEs and concentration of aniline monomer on the stability and morphology of the hybrid microparticles were studied. The obtained hybrid microparticles were characterized by SEM, FT-IR, UV-Vis, etc. Furthermore, the hybrid microparticles were deposited on glassy carbon electrode, which displayed high electrocatalytical activity toward the oxidation of dopamine(DA). The oxidized peak potential was negatively shifted with a value of 130 mV, compared with that using pure CaCO3 microparticles. The modified electrode showed good reproducibility, and the relative standard deviation(RSD) was estimated to be about 4.2% in 4.0 mmol/L DA aqueous solution (n=5). The obtained hybrid microparticles have great potential in construction of biosensors. The linear range was in the range of 0.5~10.0 mmol/L, with the detection limit of 0.2 mmol/L(3S/N).
Polyaniline(PAN) was in-situ formed around calcium carbonate(CaCO3) microparticles previously stabilized with polyelectrolyte layers (PEs), generating PAN/(PEs)6/CaCO3 hybrid microparticles. The effects of PEs and concentration of aniline monomer on the stability and morphology of the hybrid microparticles were studied. The obtained hybrid microparticles were characterized by SEM, FT-IR, UV-Vis, etc. Furthermore, the hybrid microparticles were deposited on glassy carbon electrode, which displayed high electrocatalytical activity toward the oxidation of dopamine(DA). The oxidized peak potential was negatively shifted with a value of 130 mV, compared with that using pure CaCO3 microparticles. The modified electrode showed good reproducibility, and the relative standard deviation(RSD) was estimated to be about 4.2% in 4.0 mmol/L DA aqueous solution (n=5). The obtained hybrid microparticles have great potential in construction of biosensors. The linear range was in the range of 0.5~10.0 mmol/L, with the detection limit of 0.2 mmol/L(3S/N).
2011, 28(1): 27-32
doi: 10.3724/SP.J.1095.2011.00215
Abstract:
An inorganic polymeric composite flocculant polyferric silicate sulfate (PFSS) and assistant flocculant chitosan(CTS) have been prepared. Factors that influence the synthesis and applications of the flocculants have been investigated. The composition, dosage and pH value have been discussed in terms of treating the municipal wastewater. The optimal conditions of synthesis and application have been achieved by the flocculation test of simulated wastewater and municipal wastewater. The results show that the molar ratio of Fe/Si is 1, the basicity of PFSS is 1.5, pH of the polyferric sulfate(PFS) is 2, the activating time of the polysilicate(PS) is 1.5 h; the mass ratio of PFSS/CTS is 5:1, the dosage is (20+4) mg/L, the range of pH is 6 to 9, the sedimental time is 15 min. The turbidity, chromaticity, and COD removing rate of composite flocculant PFSS-CTS reached 95.04%, 91.26%, and 83.45%, respectively, under optimized conditions.
An inorganic polymeric composite flocculant polyferric silicate sulfate (PFSS) and assistant flocculant chitosan(CTS) have been prepared. Factors that influence the synthesis and applications of the flocculants have been investigated. The composition, dosage and pH value have been discussed in terms of treating the municipal wastewater. The optimal conditions of synthesis and application have been achieved by the flocculation test of simulated wastewater and municipal wastewater. The results show that the molar ratio of Fe/Si is 1, the basicity of PFSS is 1.5, pH of the polyferric sulfate(PFS) is 2, the activating time of the polysilicate(PS) is 1.5 h; the mass ratio of PFSS/CTS is 5:1, the dosage is (20+4) mg/L, the range of pH is 6 to 9, the sedimental time is 15 min. The turbidity, chromaticity, and COD removing rate of composite flocculant PFSS-CTS reached 95.04%, 91.26%, and 83.45%, respectively, under optimized conditions.
2011, 28(1): 33-38
doi: 10.3724/SP.J.1095.2011.00204
Abstract:
ZnTiO3-TiO2 nano-composite photocatalytic materials were prepared via a Sol-Gel method and characterized by transmission electron microscope(TEM), X-ray diffractometry(XRD), UV-Vis spectrum and zeta(ζ) potential. The influences of light source and calcination temperature on the photocatalytic property of the nano-composite materials was investigated by decolorizing degradation of methylene blue(MB) solution as a probe. The results exhibit that the catalytic activity of the as-prepared material depends on the particle size, dispersibility in solution as well as the superficial charge. On the surface of the ZnTiO3-TiO2 obtained by calcinin at 600℃ for 3 h, which can disperse well in solution and has an average particle size of 60 nm and highest negative charge, decolorizing efficiency of MB solution was up to 93% under sunlight radiation for 7 h while the efficiency was just 82% under ultraviolet light radiation for same time radiation. Such efficiency can be maintained higher than 80% when the catalyst is repeatedly used for 4 times. The nano-composite material shows higher photocatalytic activity than pure TiO2 and ZnO, and has preferable photocatalytic stabilization property under sunlight.
ZnTiO3-TiO2 nano-composite photocatalytic materials were prepared via a Sol-Gel method and characterized by transmission electron microscope(TEM), X-ray diffractometry(XRD), UV-Vis spectrum and zeta(ζ) potential. The influences of light source and calcination temperature on the photocatalytic property of the nano-composite materials was investigated by decolorizing degradation of methylene blue(MB) solution as a probe. The results exhibit that the catalytic activity of the as-prepared material depends on the particle size, dispersibility in solution as well as the superficial charge. On the surface of the ZnTiO3-TiO2 obtained by calcinin at 600℃ for 3 h, which can disperse well in solution and has an average particle size of 60 nm and highest negative charge, decolorizing efficiency of MB solution was up to 93% under sunlight radiation for 7 h while the efficiency was just 82% under ultraviolet light radiation for same time radiation. Such efficiency can be maintained higher than 80% when the catalyst is repeatedly used for 4 times. The nano-composite material shows higher photocatalytic activity than pure TiO2 and ZnO, and has preferable photocatalytic stabilization property under sunlight.
2011, 28(1): 39-43
doi: 10.3724/SP.J.1095.2011.00137
Abstract:
Anatase TiO2 coatings on highly porous expanded graphite(EG) were prepared by equal volume impregnation method. The morphology of EG with and without TiO2 coatings were studied by scanning electron microscope. The XRD pattern of TiO2 power was also studied. The composite material was filled into the novel home-made photoelectric reactor to degrade textile waste water containing reactive blue. The effects of different degradation technologies, such as photocatalysis, electro-oxidation, and photoelectrocatalysis were investigated and compared. The results show that chemical oxygen demand(COD) removal and color removal efficiency of the waste water by photoelectrocatalysis using 0.1 mol/L NaCl as supporting electrolyte is 93.1% and 99.3%, respectively, which are much higher than those obtained by using only photocatalysis or electrocatalysis.
Anatase TiO2 coatings on highly porous expanded graphite(EG) were prepared by equal volume impregnation method. The morphology of EG with and without TiO2 coatings were studied by scanning electron microscope. The XRD pattern of TiO2 power was also studied. The composite material was filled into the novel home-made photoelectric reactor to degrade textile waste water containing reactive blue. The effects of different degradation technologies, such as photocatalysis, electro-oxidation, and photoelectrocatalysis were investigated and compared. The results show that chemical oxygen demand(COD) removal and color removal efficiency of the waste water by photoelectrocatalysis using 0.1 mol/L NaCl as supporting electrolyte is 93.1% and 99.3%, respectively, which are much higher than those obtained by using only photocatalysis or electrocatalysis.
2011, 28(1): 44-47
doi: 10.3724/SP.J.1095.2011.00190
Abstract:
The carbon-supported Pt-P(Pt-P/C) catalyst(m(Pt):m(P)=5:1) was prepared with NaH2 PO2 reduction method. The X-ray diffraction results indicate that the 2θ values of the Pt diffraction peaks of the Pt-P/C catalyst are slightly greater than those of the Pt/C catalyst, illustrating that P has entered into the crystal lattice of Pt and forms the Pt-P alloy. The electrochemical measurements demonstrated that the electrocatalytic performance of the Pt-P/C catalyst for the oxygen reduction is better than that of the commercial E-TEK Pt/C catalyst with 40 mV positive shift of reduction potential, which may be attributed to the P action because the average size and the relative crystallinity of the Pt-P particles in the Pt-P/C catalyst are similar to those in Pt/C catalyst.
The carbon-supported Pt-P(Pt-P/C) catalyst(m(Pt):m(P)=5:1) was prepared with NaH2 PO2 reduction method. The X-ray diffraction results indicate that the 2θ values of the Pt diffraction peaks of the Pt-P/C catalyst are slightly greater than those of the Pt/C catalyst, illustrating that P has entered into the crystal lattice of Pt and forms the Pt-P alloy. The electrochemical measurements demonstrated that the electrocatalytic performance of the Pt-P/C catalyst for the oxygen reduction is better than that of the commercial E-TEK Pt/C catalyst with 40 mV positive shift of reduction potential, which may be attributed to the P action because the average size and the relative crystallinity of the Pt-P particles in the Pt-P/C catalyst are similar to those in Pt/C catalyst.
2011, 28(1): 48-54
doi: 10.3724/SP.J.1095.2011.00251
Abstract:
Lithium methoxy oligo (oxyethylene) sulfate (LiSA (EO)n) and pentaerythritol tetrakis (2-methoxyethyl ether) (STEO) were synthesized and used for the preparation of polyethylene oxide(PEO) based polymer electrolytes. All solid-state polymer electrolytes PEO-LiSA(EO)n and PEO-LiClO4 were obtained by the solvent casting method and the ionic conductivities and lithium ion transference numbers were measured by using ac impedance and steady state current methods respectively. The influences of lithium salt structure on lithium ion transference numbers and ionic conductivities of polymer electrolytes were studied. Results showed that, comparing with LiClO4, LiSA(EO)n could enhance the ionic conductivity of polymer electrolytes and ionic conductivity decreased with increasing size of anion of lithium salt. Lithium ion transference numbers increased with increasing size of anion of lithium salt, and achieved a relatively high value of 0.35 when (PEO16+LiSA (EO)2) was used. Composed polymer electrolytes (CPEs) PEO16-LiSAEO-STEO were prepared and the effects of addition of STEO on ionic conductivities were discussed. The experimental results showed that the addition of STEO could improve the ionic conductivity of the composited polymer electrolytes effectively, the ionic conductivity of PEO16-LiSAEO-20% STEO achieved 0.5×10-4 S/cm under 25℃. The thermal properties of CPEs were investigated by DSC experiments. Results indicated that the addition of STEO could decrease the melting temperature and crystallinity of CPE, resulting in the improvement of ionic conductivity. The electrochemical stability window of PEO16-LiSAEO-20% STEO exceeded 4.4 V, which ensured the use of PEO16-LiSAEO-STEO as electrolyte materials for all solid-state rechargeable lithium ion batteries.
Lithium methoxy oligo (oxyethylene) sulfate (LiSA (EO)n) and pentaerythritol tetrakis (2-methoxyethyl ether) (STEO) were synthesized and used for the preparation of polyethylene oxide(PEO) based polymer electrolytes. All solid-state polymer electrolytes PEO-LiSA(EO)n and PEO-LiClO4 were obtained by the solvent casting method and the ionic conductivities and lithium ion transference numbers were measured by using ac impedance and steady state current methods respectively. The influences of lithium salt structure on lithium ion transference numbers and ionic conductivities of polymer electrolytes were studied. Results showed that, comparing with LiClO4, LiSA(EO)n could enhance the ionic conductivity of polymer electrolytes and ionic conductivity decreased with increasing size of anion of lithium salt. Lithium ion transference numbers increased with increasing size of anion of lithium salt, and achieved a relatively high value of 0.35 when (PEO16+LiSA (EO)2) was used. Composed polymer electrolytes (CPEs) PEO16-LiSAEO-STEO were prepared and the effects of addition of STEO on ionic conductivities were discussed. The experimental results showed that the addition of STEO could improve the ionic conductivity of the composited polymer electrolytes effectively, the ionic conductivity of PEO16-LiSAEO-20% STEO achieved 0.5×10-4 S/cm under 25℃. The thermal properties of CPEs were investigated by DSC experiments. Results indicated that the addition of STEO could decrease the melting temperature and crystallinity of CPE, resulting in the improvement of ionic conductivity. The electrochemical stability window of PEO16-LiSAEO-20% STEO exceeded 4.4 V, which ensured the use of PEO16-LiSAEO-STEO as electrolyte materials for all solid-state rechargeable lithium ion batteries.
2011, 28(1): 55-59
doi: 10.3724/SP.J.1095.2011.00140
Abstract:
Electrodeposition of Pb on polycrystalline Cu surfaces has been investigated by cyclic voltammetry (CV) and in-situ spectroscopic ellipsometry(SE). The ellipsometric parameters Ψ and Δ peak corresponded to both underpotential deposition (UPD) and bulk deposition peak potentials. The "substrate-solution" interface structure was described with a single-layer model,(substrate Cu-deposition Pb layer) and the thicknesses of Pb layer for different scan potentials were obtained by fitting experimental data with the model. Fitting results showed that Pb electrodeposition on the Cu electrode was with three different deposition rates,-0.20~-0.35 V,0.003 nm/mV;-0.35~-0.48V,0.025 nm/mV;-0.48~-0.60 V,0.116 nm/mV. Based on the fitting results, three stages, which were formation of UPD layer, transitional period between the UPD and bulk deposition and formation of bulk deposition layer were proposed for the electrodeposition process of copper in the Pb2+ solution.
Electrodeposition of Pb on polycrystalline Cu surfaces has been investigated by cyclic voltammetry (CV) and in-situ spectroscopic ellipsometry(SE). The ellipsometric parameters Ψ and Δ peak corresponded to both underpotential deposition (UPD) and bulk deposition peak potentials. The "substrate-solution" interface structure was described with a single-layer model,(substrate Cu-deposition Pb layer) and the thicknesses of Pb layer for different scan potentials were obtained by fitting experimental data with the model. Fitting results showed that Pb electrodeposition on the Cu electrode was with three different deposition rates,-0.20~-0.35 V,0.003 nm/mV;-0.35~-0.48V,0.025 nm/mV;-0.48~-0.60 V,0.116 nm/mV. Based on the fitting results, three stages, which were formation of UPD layer, transitional period between the UPD and bulk deposition and formation of bulk deposition layer were proposed for the electrodeposition process of copper in the Pb2+ solution.
2011, 28(1): 60-65
doi: 10.3724/SP.J.1095.2011.00150
Abstract:
Fe-Ni-S alloy film was prepared on red copper foil by electrodeposition from a acidic bath containing boric acid as a buffer agent and sodium citrate as a complexing agent. The effects of the bath composition, and the deposition parameters on the surface morphology and the composition of the alloy coating were studied by SEM and EDS. As a result, a smooth coating with no crack and little stress was obtained from the plating bath by adding 2 g/L saccharin and 0.4 g/L 1,4-butynediol. The cathodic current density and the plating bath pH have little effect on the coating composition, but the temperature has great effect. Fe73Ni9.5S17.5 film was prepared in optimized plating conditions, and XRD analysis showed that the coating structure is amorphous. The film has good soft magnetic performances with higher saturation magnetization (Ms≈876.25 kA/m) and lower coercivity(Hc≈4.96 kA/m) at room temperature. Cyclic voltammetry and the cathodic polarization curves indicated that thiourea can promote the co-deposition of Fe-Ni-S alloy.
Fe-Ni-S alloy film was prepared on red copper foil by electrodeposition from a acidic bath containing boric acid as a buffer agent and sodium citrate as a complexing agent. The effects of the bath composition, and the deposition parameters on the surface morphology and the composition of the alloy coating were studied by SEM and EDS. As a result, a smooth coating with no crack and little stress was obtained from the plating bath by adding 2 g/L saccharin and 0.4 g/L 1,4-butynediol. The cathodic current density and the plating bath pH have little effect on the coating composition, but the temperature has great effect. Fe73Ni9.5S17.5 film was prepared in optimized plating conditions, and XRD analysis showed that the coating structure is amorphous. The film has good soft magnetic performances with higher saturation magnetization (Ms≈876.25 kA/m) and lower coercivity(Hc≈4.96 kA/m) at room temperature. Cyclic voltammetry and the cathodic polarization curves indicated that thiourea can promote the co-deposition of Fe-Ni-S alloy.
2011, 28(1): 66-71
doi: 10.3724/SP.J.1095.2011.00078
Abstract:
Gadolinium-doped TiO2/activated carbon fibre composite(TG/ACF) was prepared from TiCl4 and Gd(NO3)3·6H2O by acid-catalyzed hydrolysis method, then it was loaded on active carbon fiber (ACF) surface by impregnation. The photocatalytic activity was evaluated by degradation of gaseous benzene. XRD, FTIR and GC-MS were used to characterize the obtained composite. The results showed that Gd-doping could inhibit the growth of TiO2 crystallite. The photocatalytic activity of gadolinium-doped TiO2/ACF was affected by the added amount of Gd and dip-coating times. When the mass fraction of doped-gadolinium was 0.48% and dip-coating for 2 times, the composite exhibited the highest photocatalytic activity for benzene removal. No quinine compound was detected on gadolinium-doped TiO2/ACF composite surface after photocatalytic oxidation of benzene. The doped-Gd could slow down the deactivation of the catalyst, and the catalyst remained high activity after 100 min of usage.
Gadolinium-doped TiO2/activated carbon fibre composite(TG/ACF) was prepared from TiCl4 and Gd(NO3)3·6H2O by acid-catalyzed hydrolysis method, then it was loaded on active carbon fiber (ACF) surface by impregnation. The photocatalytic activity was evaluated by degradation of gaseous benzene. XRD, FTIR and GC-MS were used to characterize the obtained composite. The results showed that Gd-doping could inhibit the growth of TiO2 crystallite. The photocatalytic activity of gadolinium-doped TiO2/ACF was affected by the added amount of Gd and dip-coating times. When the mass fraction of doped-gadolinium was 0.48% and dip-coating for 2 times, the composite exhibited the highest photocatalytic activity for benzene removal. No quinine compound was detected on gadolinium-doped TiO2/ACF composite surface after photocatalytic oxidation of benzene. The doped-Gd could slow down the deactivation of the catalyst, and the catalyst remained high activity after 100 min of usage.
2011, 28(1): 72-76
doi: 10.3724/SP.J.1095.2011.00246
Abstract:
Effects of the dispersant, mass fraction of styrene-acrylic acid random copolymer(MOTAS), mass fraction of ethanol on the dispersion stability of hexaflumuron suspension produced by a solvent displacement technique were studied by means of measuring the average particle size and Zeta potential analysis. It has been found that the dispersive effect of MOTAS on the suspension was greater than others under the same condition. Under the condition of 1% mass fraction of MOTAS, Dav is the minimal, Zeta potential is the maximal and the dispersion stability is the best. The dispersion stability of the hexaflumuron suspension can be greatly enhanced when the ethanol was added. The dispersion stability attained best in solution containing about 31.2% mass fraction of ethanol.
Effects of the dispersant, mass fraction of styrene-acrylic acid random copolymer(MOTAS), mass fraction of ethanol on the dispersion stability of hexaflumuron suspension produced by a solvent displacement technique were studied by means of measuring the average particle size and Zeta potential analysis. It has been found that the dispersive effect of MOTAS on the suspension was greater than others under the same condition. Under the condition of 1% mass fraction of MOTAS, Dav is the minimal, Zeta potential is the maximal and the dispersion stability is the best. The dispersion stability of the hexaflumuron suspension can be greatly enhanced when the ethanol was added. The dispersion stability attained best in solution containing about 31.2% mass fraction of ethanol.
2011, 28(1): 77-82
doi: 10.3724/SP.J.1095.2011.00200
Abstract:
Compound[InAsS4(2,2'-bipy)]2, which contains AsS43- (As(Ⅲ)) unit, was synthesized by the hydrothermal method. The compound crystalizes in monoclinic space group P21/c with a=0.89799(9) nm, b=2.1794(2) nm, c=1.43736(14) nm, β=91.274(2)°, V=2.8123(5) nm3. In this compound, the AsS43-(As(Ⅲ)) unitis stabilized by metal-amino complex[In(2,2'-bipy)]3+. The effect of metal charge on the formation of this product was discussed and the band gap of the as-synthesized semiconductor is found to be 1.35 eV.
Compound[InAsS4(2,2'-bipy)]2, which contains AsS43- (As(Ⅲ)) unit, was synthesized by the hydrothermal method. The compound crystalizes in monoclinic space group P21/c with a=0.89799(9) nm, b=2.1794(2) nm, c=1.43736(14) nm, β=91.274(2)°, V=2.8123(5) nm3. In this compound, the AsS43-(As(Ⅲ)) unitis stabilized by metal-amino complex[In(2,2'-bipy)]3+. The effect of metal charge on the formation of this product was discussed and the band gap of the as-synthesized semiconductor is found to be 1.35 eV.
2011, 28(1): 83-87
doi: 10.3724/SP.J.1095.2011.00124
Abstract:
Water-soluble polysaccharide B(BRP-B) in Blumea riparia(BI.) DC. was extracted and purified by using membrane separation, discoloration on diethylaminoethyl(DEAE)-cellulose, and sephadex column chromatography of G10 and G50. Results from high-performance gel permeation chromatography (HPGPC) showed that the obtained BRP-B has a narrow-distributed molecular mass, with the number average molecular mass and mass average molecular mass as 2654 and 2716, respectively. The drug activity test based on plasma recalcification as the index showed that BRP-B with the optimal concentration of 6.25×10-2 g/L had the strongest procoagulant activity, the coagulation time was 248.52 s, and the inhibition rate of coagulation time was 22.42%. In particularly, BRP-B with concentration of 1.67×10-2, 1.97×10-2 and 2.85×10-2 g/L could significantly enhance the frequency of uterus muscle.
Water-soluble polysaccharide B(BRP-B) in Blumea riparia(BI.) DC. was extracted and purified by using membrane separation, discoloration on diethylaminoethyl(DEAE)-cellulose, and sephadex column chromatography of G10 and G50. Results from high-performance gel permeation chromatography (HPGPC) showed that the obtained BRP-B has a narrow-distributed molecular mass, with the number average molecular mass and mass average molecular mass as 2654 and 2716, respectively. The drug activity test based on plasma recalcification as the index showed that BRP-B with the optimal concentration of 6.25×10-2 g/L had the strongest procoagulant activity, the coagulation time was 248.52 s, and the inhibition rate of coagulation time was 22.42%. In particularly, BRP-B with concentration of 1.67×10-2, 1.97×10-2 and 2.85×10-2 g/L could significantly enhance the frequency of uterus muscle.
2011, 28(1): 88-93
doi: 10.3724/SP.J.1095.2011.00161
Abstract:
A spectrophotometric method has been set up to determine cefotaxime sodium using potassium ferricyanide as the spectroscopic probe reagent. With the presence of potassium ferricyanide, the degradation product of cefotaxime sodium can reduce Fe3+ to Fe2+ at pH 3.0, which facilitate the formation of soluble Prussian Blue (KFeⅢ[FeⅡ(CN)6]). The absorbance of soluble Prussian Blue is measured at its absorption maximum of 730 nm and the amount of cefotaxime sodium can be indirectly calculated. Under optimized conditions, a good linear relationship is obtained in the range of 0.040~24 mg/L of cefotaxime sodium. The linear regression equation is A=0.05088+0.2166ρ(mg/L) with linear correlation coefficient of 0.9986. The detection limit and relative standard deviation are 0.01 mg/L and 1.36%, respectively. Tthe apparent molar absorption coefficient of indirect determination of cefotaxime sodium is 2.3×105 L/(mol·cm). This method has been successfully applied to the determination of cefotaxime sodium in pharmaceutical and serum samples.
A spectrophotometric method has been set up to determine cefotaxime sodium using potassium ferricyanide as the spectroscopic probe reagent. With the presence of potassium ferricyanide, the degradation product of cefotaxime sodium can reduce Fe3+ to Fe2+ at pH 3.0, which facilitate the formation of soluble Prussian Blue (KFeⅢ[FeⅡ(CN)6]). The absorbance of soluble Prussian Blue is measured at its absorption maximum of 730 nm and the amount of cefotaxime sodium can be indirectly calculated. Under optimized conditions, a good linear relationship is obtained in the range of 0.040~24 mg/L of cefotaxime sodium. The linear regression equation is A=0.05088+0.2166ρ(mg/L) with linear correlation coefficient of 0.9986. The detection limit and relative standard deviation are 0.01 mg/L and 1.36%, respectively. Tthe apparent molar absorption coefficient of indirect determination of cefotaxime sodium is 2.3×105 L/(mol·cm). This method has been successfully applied to the determination of cefotaxime sodium in pharmaceutical and serum samples.
2011, 28(1): 94-100
doi: 10.3724/SP.J.1095.2011.00101
Abstract:
An imidazolinyl-quaternary ammonium salts inhibitor (MIQ) with multi-activated sites was synthesized from p-(dimethylamino)-benzoic acid, diethylenetriamine and benzyl chloride. The synthesized inhibitor was characterized by FTIR. The anti-corrosion performance of the compound on mild steel was investigated in 6% hydrochloric acid using a mass loss method. Effecting factors of the anti-corrosion performance such as concentration, temperature and contact time were discussed. The results show that the inhibitive efficiency of the inhibitor can reach 97% when the concentration of MIQ is 0.5% and the inhibition efficiency undergoes a decrease trend with the increase of temperature and immersion time. After combined with KSCN, KI and so on, the resultant complexes significantly improve the inhibition efficiency. The adsorption of MIQ on the steel follows a Langmuir adsorption isotherm. The absorbed MIQ forms a thin film on of the mild steel and efficiently prevents its direct contact with the acidic detergent reagent.
An imidazolinyl-quaternary ammonium salts inhibitor (MIQ) with multi-activated sites was synthesized from p-(dimethylamino)-benzoic acid, diethylenetriamine and benzyl chloride. The synthesized inhibitor was characterized by FTIR. The anti-corrosion performance of the compound on mild steel was investigated in 6% hydrochloric acid using a mass loss method. Effecting factors of the anti-corrosion performance such as concentration, temperature and contact time were discussed. The results show that the inhibitive efficiency of the inhibitor can reach 97% when the concentration of MIQ is 0.5% and the inhibition efficiency undergoes a decrease trend with the increase of temperature and immersion time. After combined with KSCN, KI and so on, the resultant complexes significantly improve the inhibition efficiency. The adsorption of MIQ on the steel follows a Langmuir adsorption isotherm. The absorbed MIQ forms a thin film on of the mild steel and efficiently prevents its direct contact with the acidic detergent reagent.
2011, 28(1): 101-106
doi: 10.3724/SP.J.1095.2011.00174
Abstract:
The detection of folic acid by a fluorescent energy transfer method has been developed. In the folic acid-KMnO4-Eu3+-H2O2 system with the presence of HAc-NaAc buffer solution(pH=4.7,0.2 mol/L), the folic acid can be oxidized by KMnO4 with the presence of H2O2 and converted into the purine of butterfly-6-carboxyl acid, which can coordinate with Eu3+ forming a complex. The experimental conditions including the concentration of buffer solution and pH value, choice of oxidant, the temperature and heating time, the concentration of Eu3+, etc., were optimized. This system can emit the characteristic fluorescence of Eu3+ through an intra-molecule energy transfer process. The fluorescent intensity is in proportional to the concentration of folic acid in the range of 4×10-8~4×10-5 mol/L with correlation coefficient of 0.9902. The detection limit is found to be 1.2×10-8 mol/L. The developed method has been successfully applied to the determination of folic acid in the actual samples.
The detection of folic acid by a fluorescent energy transfer method has been developed. In the folic acid-KMnO4-Eu3+-H2O2 system with the presence of HAc-NaAc buffer solution(pH=4.7,0.2 mol/L), the folic acid can be oxidized by KMnO4 with the presence of H2O2 and converted into the purine of butterfly-6-carboxyl acid, which can coordinate with Eu3+ forming a complex. The experimental conditions including the concentration of buffer solution and pH value, choice of oxidant, the temperature and heating time, the concentration of Eu3+, etc., were optimized. This system can emit the characteristic fluorescence of Eu3+ through an intra-molecule energy transfer process. The fluorescent intensity is in proportional to the concentration of folic acid in the range of 4×10-8~4×10-5 mol/L with correlation coefficient of 0.9902. The detection limit is found to be 1.2×10-8 mol/L. The developed method has been successfully applied to the determination of folic acid in the actual samples.
2011, 28(1): 107-112
doi: 10.3724/SP.J.1095.2011.00195
Abstract:
In 5.0 mol/L HCl buffer solution, phosphowolframic acid (Pwa) could react with moxifloxacin (MXFX) and gatifloxacin (GTF) fluoroquinolone antibiotics (FLQs) to form 1:1 ion-associated complexes respectively. The reactions resulted in great enhancement of resonance Rayleigh scattering(RRS) and new RRS bands appear. The reaction products of the two drugs had similar spectral characteristics, and the maximum RRS wavelength was located at 320 nm. The intensities of RRS are proportional to the concentration of antibiotics, the linearity ranges of two fluoroquinolone antibiotics are 0.025~6.0 mg/L (MXFX) and 0.023~9.0 mg/L(GTF), respectively. Therefore, a new method for determination of the drugs could be developed and applied to the determination of FLQs in capsules and human urine samples. The reaction mechanism and the reasons for RRS enhancement of the system were investigated.
In 5.0 mol/L HCl buffer solution, phosphowolframic acid (Pwa) could react with moxifloxacin (MXFX) and gatifloxacin (GTF) fluoroquinolone antibiotics (FLQs) to form 1:1 ion-associated complexes respectively. The reactions resulted in great enhancement of resonance Rayleigh scattering(RRS) and new RRS bands appear. The reaction products of the two drugs had similar spectral characteristics, and the maximum RRS wavelength was located at 320 nm. The intensities of RRS are proportional to the concentration of antibiotics, the linearity ranges of two fluoroquinolone antibiotics are 0.025~6.0 mg/L (MXFX) and 0.023~9.0 mg/L(GTF), respectively. Therefore, a new method for determination of the drugs could be developed and applied to the determination of FLQs in capsules and human urine samples. The reaction mechanism and the reasons for RRS enhancement of the system were investigated.
2011, 28(1): 113-117
doi: 10.3724/SP.J.1095.2011.00243
Abstract:
Using the chromophore base of benzene sulfonate in sodium dodecyl benzene sulfonate(SDBS), the aggregation property of SDBS with non-ionic surfactant TritonX-100 in aqueous solution was studied by fluorescence. Results show there are two turning points in the variation curve of fluorescence intensity I as a function of concentration, which is the critical micelle concentration and the concentration at which the micelle shape changed, respectively. The interaction parameter βM between SDBS and TritonX-100 was calculated by the formula of mixed micelle interaction. The results show there is synergism and strong interaction between them.
Using the chromophore base of benzene sulfonate in sodium dodecyl benzene sulfonate(SDBS), the aggregation property of SDBS with non-ionic surfactant TritonX-100 in aqueous solution was studied by fluorescence. Results show there are two turning points in the variation curve of fluorescence intensity I as a function of concentration, which is the critical micelle concentration and the concentration at which the micelle shape changed, respectively. The interaction parameter βM between SDBS and TritonX-100 was calculated by the formula of mixed micelle interaction. The results show there is synergism and strong interaction between them.
2011, 28(1): 118-120
doi: 10.3724/SP.J.1095.2011.00216
Abstract:
Esterification reaction of boric acid, pinacol and cyclohexanol has been studied in ionic liquids (IL), including 1-methyl-2-pyrrolidonium hydrogen sulfate([Hnmp]HSO4), 1-butyl-3-methylimidazolium tetrafluoroborate([Bmim]BF4) and 1-butyl-3-methylimidazolium hexafluorophosphate([Bmim]PF6). The influences of the types of ionic liquids, reaction temperature, reaction time and molar ratio of reactants to IL on the yields of 2-cyclohexyloxy-4,4,5,5-tetramethyl-[1,3,2]dioxaborolan have been investigated. The results showed that under the optimized conditions[n (boric acid):n (pinacol):n (cyclohexanol):n([Hnmp]HSO4)=1:1:1:1, 70℃ and 4 h], the yield of 2-cyclohexyloxy-4,4,5,5-tetramethyl-[1,3,2] dioxaborolan could reach up to 72.5%. The ionic liquid can be used repeatedly for four times without remarkable loss of the catalytic activity.
Esterification reaction of boric acid, pinacol and cyclohexanol has been studied in ionic liquids (IL), including 1-methyl-2-pyrrolidonium hydrogen sulfate([Hnmp]HSO4), 1-butyl-3-methylimidazolium tetrafluoroborate([Bmim]BF4) and 1-butyl-3-methylimidazolium hexafluorophosphate([Bmim]PF6). The influences of the types of ionic liquids, reaction temperature, reaction time and molar ratio of reactants to IL on the yields of 2-cyclohexyloxy-4,4,5,5-tetramethyl-[1,3,2]dioxaborolan have been investigated. The results showed that under the optimized conditions[n (boric acid):n (pinacol):n (cyclohexanol):n([Hnmp]HSO4)=1:1:1:1, 70℃ and 4 h], the yield of 2-cyclohexyloxy-4,4,5,5-tetramethyl-[1,3,2] dioxaborolan could reach up to 72.5%. The ionic liquid can be used repeatedly for four times without remarkable loss of the catalytic activity.
2011, 28(1): 121-122
doi: 10.3724/SP.J.1095.2011.00234
Abstract:
Chiral 3,3'-substituted 1,1'-bi-2-napthol(BINOL) derivatives were synthesized from BINOL. The asymmetric addition of phenylacetylene and benzaldehyde in the presence of the BINOL derivative and diethyl zinc afforded the corresponding propargylic alcohols with 73% yield and 40% enatiomeric excess.
Chiral 3,3'-substituted 1,1'-bi-2-napthol(BINOL) derivatives were synthesized from BINOL. The asymmetric addition of phenylacetylene and benzaldehyde in the presence of the BINOL derivative and diethyl zinc afforded the corresponding propargylic alcohols with 73% yield and 40% enatiomeric excess.
