The Synthesis And Characterization Of Newly MOFs As Solid Phase Extraction Adsorbent And Its Performance Research

Metal organic Frameworks（MOFs）has many excellent merits such as large specific surface area and porosity,adjustable pore size and topology structure,the advantages of good solvent stability and thermal stability.Therefore,it is widely used to gas adsorption and storage,catalysis,sensors and so on.Furthermore,MOFs is applied to the sample pretreatment in recent years.This thesis aims at synthetizing novel MOFs materials and screening novel MOFs materials with high adsorbability and studying the enrichment efficiency of PAHs,establishing SPE-HPLC analytical method of PAHs and optimizing enrichment factors to improve the adsorption efficiency of trace PAHs in water.It consists three chapters.In chapter one,Lanthanum-diphenyltriacid MOFs materials was synthetized,the surface composition and structure of the adsorbent were characterized in detail using Scanning Electron Microscope（SEM）,Thermo-gravimetric Analysis（TGA）and X-ray Diffraction（XRD）.The SPE-HPLC analytical method was established using the home-made MOFs materials as adsorbent for the analysis of eight kinds of PAHs including naphthalene,acenaphthylene,acenaphthene,phenanthrene,anthracene,fluoranthene,pyrene and benzanthracene in water.Firstly,experimental conditions were optimized to determine the parameters including the velocity and proportion of the mobile phase.Then,the influence of the conditions in Solid Phase Extraction were investigated which are sample volume,mass of absorbent,amount of eluent,pH and dilution ratio of standard samples.The linear correlation coefficient was above 0.9916.The limits of detection for the eight kinds of analysis ranged from 0.07μg/L to 29.6μg/L.The precision ranged from 2.7%to 24.3%.This method was successfully applied to the analysis of samples with 85%-100%recoveries.And the peak area was compared with which obtained by C₁₈ column.In chapter two,Copper-2-amino terephthalic acid MOFs with different proportion of metal ion and organic ligand was synthetized,then,the ratio of 2:1 of metal ion and organic ligand was confirmed as adsorbent,and the surface composition and structure of the adsorbent were characterized in detail using Scanning Electron Microscope（SEM）,Thermo-gravimetric Analysis（TGA）and X-ray Diffraction（XRD）.The SPE-HPLC analytical method was established using the home-made MOFs materials as adsorbent for the analysis of seven kinds of PAHs including naphthalene,acenaphthylene,acenaphthene,anthracene,fluoranthene,pyrene and benzanthracene in water.Firstly,experimental conditions were optimized to determine the parameters including the velocity and proportion of the mobile phase.Then,the influence of the conditions in Solid Phase Extraction were investigated which are sample volume,mass of absorbent,amount of eluent,pH and dilution ratio of standard samples.The linear correlation coefficient was above 0.9919.The limits of detection for the seven kinds of analysis ranged from0.03μg/L to 0.09μg/L.The precision ranged from 3.3%to 11.3%.This method was successfully applied to the analysis of samples with 85%-110%recoveries.And the peak area was compared with which obtained by C₁₈ column.In chapter three,Lanthanum-2-amino terephthalic acid MOFs material was synthetized with the ratio 2:1 of metal ion and organic ligand as adsorbent,and the surface composition and structure of the adsorbent were characterized in detail using Scanning Electron Microscope（SEM）,Thermo-gravimetric Analysis（TGA）and X-ray Diffraction（XRD）.The SPE-HPLC analytical method was established using the home-made MOFs materials as adsorbent for the analysis of seven kinds of PAHs including naphthalene,acenaphthylene,acenaphthene,anthracene,fluoranthene,pyrene and benzanthracene in water.Firstly,experimental conditions were optimized to determine the parameters including the velocity and proportion of the mobile phase.Then,the influence of the conditions in Solid Phase Extraction were investigated which are sample volume,mass of absorbent,amount of eluent,pH and dilution ratio of standard samples.The linear correlation coefficient was above 0.9926.The limits of detection for the seven kinds of analysis ranged from0.03μg/L to 0.20μg/L.The precision ranged from 7.3%to 19.1%.This method was successfully applied to the analysis of samples with 80%-116%recoveries.And the peak area was compared with which obtained by C₁₈ column.