[Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From...[Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amount of PAHs in urban sewage was determined.[Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 solid-phase extraction column,methylene dichloride as elution solvent,15 ml elution volume,2 ml/min elution speed,5 ml/min loading speed,1 000 ml water with 200 ml methanol loading volume.Under the optimized extraction conditions,the recovery was high,namely 76.3%-105.2%;relative standard deviation was 3.8%-6.0%,showing good precision;detection limit was low,only 0.000 8-0.048 0 μg/L.[Conclusion] This method is user-friendly,with high sensitivity and good precision,and suitable for continuous determination of a large volume of water samples.展开更多
For purpose of purification and enrichment, environmental samples usually need to be pretreated before analysis because of low concentration of residual organic matters. Solid-phase extraction （SPE） is one of the fr...For purpose of purification and enrichment, environmental samples usually need to be pretreated before analysis because of low concentration of residual organic matters. Solid-phase extraction （SPE） is one of the frequently used methods of pretreatment. This article introduces the methodological principle and flow channel of SPE as well as the categories of frequently used small extraction column, analyzes the application of online SPE technology in environmental analysis, generalizes the advantages of online SPE and sets forth its developmental trend.展开更多
The uniform zirconia nanoparticle multilayers/micrometer-sized silica particle(ZrO 2/SiO 2) was prepared for HPLC support material by layer-by-layer(LbL) self-assembly technique. XRD pattern shows that the crystalline...The uniform zirconia nanoparticle multilayers/micrometer-sized silica particle(ZrO 2/SiO 2) was prepared for HPLC support material by layer-by-layer(LbL) self-assembly technique. XRD pattern shows that the crystalline of nanometer particles on the surface is pure tetragonal zirconia, with a diameter of 13^9 nm. The specific surface area, pore volume and pore size of the material are 172.53 m 2/g, 0.378 4 cm 3/g, and 8.5 nm, respectively. The novel support not only has the mechanical strength and chemical stability of zirconia, but also has the good chromatographic features such as larger surface area, better permeability, less background pressure.展开更多
The surface properties of zirconia-based supports,ZrO-2/SiO-2 and ZrO-2,were compared.ZrO-2/SiO-2 prepared by layer-by-layer self-assembly(LbL SA) technique showed more favorable characteristics for HPLC applications ...The surface properties of zirconia-based supports,ZrO-2/SiO-2 and ZrO-2,were compared.ZrO-2/SiO-2 prepared by layer-by-layer self-assembly(LbL SA) technique showed more favorable characteristics for HPLC applications compared with ZrO-2 prepared by modified oil-emulsion method.The specific surface area and pore volume of ZrO-2/SiO-2 were about 18 and 20 times of those of ZrO-2 respectively.The pore of ZrO-2/SiO-2 support was ideal cylindrical shape,but ZrO-2 support had some \!ink bottle\" shaped-pores which was unfavorable for HPLC separations.Pore size distribution of ZrO-2/SiO-2 supports was more uniform than that of ZrO-2 supports.展开更多
基金Supported by National Science and Technology Key Project of Water Pollution Control and Management (2012ZX07209-003)
文摘[Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amount of PAHs in urban sewage was determined.[Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 solid-phase extraction column,methylene dichloride as elution solvent,15 ml elution volume,2 ml/min elution speed,5 ml/min loading speed,1 000 ml water with 200 ml methanol loading volume.Under the optimized extraction conditions,the recovery was high,namely 76.3%-105.2%;relative standard deviation was 3.8%-6.0%,showing good precision;detection limit was low,only 0.000 8-0.048 0 μg/L.[Conclusion] This method is user-friendly,with high sensitivity and good precision,and suitable for continuous determination of a large volume of water samples.
文摘For purpose of purification and enrichment, environmental samples usually need to be pretreated before analysis because of low concentration of residual organic matters. Solid-phase extraction （SPE） is one of the frequently used methods of pretreatment. This article introduces the methodological principle and flow channel of SPE as well as the categories of frequently used small extraction column, analyzes the application of online SPE technology in environmental analysis, generalizes the advantages of online SPE and sets forth its developmental trend.
文摘The uniform zirconia nanoparticle multilayers/micrometer-sized silica particle(ZrO 2/SiO 2) was prepared for HPLC support material by layer-by-layer(LbL) self-assembly technique. XRD pattern shows that the crystalline of nanometer particles on the surface is pure tetragonal zirconia, with a diameter of 13^9 nm. The specific surface area, pore volume and pore size of the material are 172.53 m 2/g, 0.378 4 cm 3/g, and 8.5 nm, respectively. The novel support not only has the mechanical strength and chemical stability of zirconia, but also has the good chromatographic features such as larger surface area, better permeability, less background pressure.
文摘The surface properties of zirconia-based supports,ZrO-2/SiO-2 and ZrO-2,were compared.ZrO-2/SiO-2 prepared by layer-by-layer self-assembly(LbL SA) technique showed more favorable characteristics for HPLC applications compared with ZrO-2 prepared by modified oil-emulsion method.The specific surface area and pore volume of ZrO-2/SiO-2 were about 18 and 20 times of those of ZrO-2 respectively.The pore of ZrO-2/SiO-2 support was ideal cylindrical shape,but ZrO-2 support had some \!ink bottle\" shaped-pores which was unfavorable for HPLC separations.Pore size distribution of ZrO-2/SiO-2 supports was more uniform than that of ZrO-2 supports.
