The Application Of Comolex Gel Membrane Micro Solid Phase Extraction In The Analysis Of Polybrominated Biphenyl Ether

With the rapid development of modern science and technology and thecontinuous advancement of society, the complexity of component, low concentrationof the target analyte and the stability depending on places and times in environmentalsamples, have put forward not only new requirements for analytical chemistry, butalso present particular challenge for new adsorbent materials of selective and high inextracting efficiency.Currently, PBDEs are distributed into all compartments of environment,including air, water, soil, milk, fish and human tissue. The migration andtransformation in environment and the related control measures is receiving people’sattention increasingly because of the persistence, bioaccumulation and potentialbiotoxicity of PBDEs. There’re traditional method such as Soxhlet Extraction,Accelerated Solvent Extraction and Solid Phase Extraction, which’re time andsolvents consumption and also complicated purification and concentration. From theenvironmental point of view as well as taking into account the rules of GreenChemistry, there’re main reasons for carrying out research on developing novelmicroextraction techniques. Micro solid-phase extraction is the new pretreatmenttechnology that based on the Solid Phase Extraction. Metal complex materials havereceived great interest in modern analytical chemistry because of their potentialanalytical applications with high surface area, the availability of in-pore functionalityand structure tailoring. Combine the specialty of Micro solid-phase extraction and thedvantages of metal complex, the thesis is comprised of the following four parts:Part one is the synthesis and characterization of9complexes based on theassemble of aromatic carboxylic and pyridine acid ligands with metal ions. It trun thatthe9complexes are the exactly compound reported in the literature from the XRDresults.Part two is the comparison with the9complexes about the ability for thepreconcentration of PBDEs in water and soil samples. It turn that the complex[Ag5（pydc）₂（CN）]_nshow the best enrichment in extracting efficiency. Then, amicro-solid-phase extraction device through the sol-gel method assembled with aMOFs-Gel-Membrane was developed.Part three is the application of MOFs-Gel-Membrane-μ-SPE for determination ofseven PBDEs in soil by coupling with gas chromatography-electron capture detector.Under the optimized conditions, the linearities for seven PBDEs were1⁵00ng/g.The method detection limits were in the range of0.08and2.6ng/g, and the recoveryof seven PBDEs were in the range of93.7and102%. Finally, the proposed methodwas successfully applied to the extraction and determination of PBDEs incontaminated site samples and certified reference materials, and it was demonstrated that the recovery of the former is in61.1⁸4.8%and the concentration of BDE-47,99,100are close to the standard except the other in certified reference materials.Part four is the application of MOFs-Gel-Membrane-μ-SPE for determination ofseven PBDEs in water. Variables affecting the extraction efficiency were investigated,including the4mg amount of the MOFs,60℃of extraction temperature,50min ofextraction time and15min of desorption time. Under the optimized conditions, therecovery of seven PBDEs were in the range of74.9and98.1%, and the relativestandard deviations were between3.3and5.7%. Limits of detection were less than4.7ng/L for all seven PBDEs. The proposed method was successfully applied to theextraction and determination of PBDEs in wastewater samples, and it turned that acertain amounts of PBDEs occured in the wastewater.