有机硅改性聚氨酯固相微萃取涂层的研制及应用

Preparing and application of siloxane-polyurethane copolymer as solid-phase microextraction coating

合成了作为固相微萃取(SPME)涂层的有机硅-聚氨酯共聚物,考察了该共聚物的物理性能;制备了萃取头并观察了萃取头的微观形貌,制作了SPME装置;用顶空萃取法对水中芳香化合物进行了萃取实验。实验结果表明:有机硅-聚氨酯共聚物固相微萃取涂层最高使用温度为250℃;萃取头涂层表面涂渍平整,涂层内硅(Si)元素分布均匀;涂层对水中苯、氯苯、硝基苯萃取的色谱峰高与浓度线性关系良好,苯∶H1=1.527C1+0.1435,R12=0.9875、氯苯∶H2=1.746C2+0.2679,R22=0.9874、硝基苯∶H3=1.254C3+1.0203,R32=0.9797,苯、氯苯、硝基苯的检出限分别为1.02、1.56和1.31μg·L-1。结果令人满意。

In this paper, siloxane-polyurethane copolymer was synthesized and applied to solid-phase microextraction coating. The structure of the polymer as SPME adsorbent was studied by IR and it＇s thermal stability, viscosity and adhesion were tested.The surface appearances of self-prepared riders for solid-phase mieroextraetion was investigated. The SPME equipment was made by refitting commercial SPME equipment （Supelco U.S.A.）.The coating was applied to detect and analyse benzene,chlorbenzenes and nitrobenzenes in water. The experiment results indicated that behaviours of the polymer coating were good.The maximum recommended temperature of coating was 250℃. SEM image of solid-phase fiber showed that surface appearance of fiber was sleek and neat; EDS surface scan of silicon on fiber showed that silicon on the surface of fiber was equally distributed. The data determined showed that the coating has particular property for extracting the aromatic compounds. The linearity relation between the concentration of benzene and chromatography peak height was H1=1.527C1＋0.1435, correlation efficient （R1^2 ） was 0.9875;The linearity relation between the concentration of chlorobenzene and relative peak height was H2= 2 1.746C2＋0.2679, correlation efficient （R2^2） was 0.9874; The linearity relation between the concentration of nitroben zene and relative peak height was H3=1.254C3＋1.0203, correlation efficient（R3^2） was 0.9797. The minimum detection limit for benzene ,chlorobenzene and nitrobenzene were 1.02,1.56 and 1.31 μ g·L^-1 respectively.