Preparation And Performance Study Of Polystyrene-methacrylic/Zirconia Packing For SPE

Solid phase extraction(SPE) was developed from liquid-solid extraction and column liquidchromatography technology.The process of solid phase extraction is that target compoundsare selective adsorbed by solid phase extraction packing and desorbed by eluant.In the process,target compounds are purified, separated and concentrated. SPE has many features such assolvent dosage small, short operation time, less interference substances, etc. Therefore, it canbe used to preproccess trace target compounds in complex samples. And it has goodreproducibility. SPE can be used in many analytical methods such as liquid chromatography(LC), gas chromatography (GC), inductively coupled plasma emission spectrometer(ICP-AES), infrared spectra (IR). Therefore, SPE has been widely used.In this paper, distributed evenly zirconia microspheres were prepared with zirconiumoxychloride and ammonia by polymerization induced colloid aggregation method. Thesurface of zirconia microspheres were modified by titanate coupling agent, then its surfacehas the carbon-carbon double bond groups. Through radical polymerization, styrene,divinylbenzene, methacrylic acid and modified zirconia surface’s double bond werepolymerized, polystyrene-methacrylic acid/zirconia solid phase extraction packing wasobtained (Initiator is BPO, dispersant is PVA). The elementary composition and microcosmicmorphology of the material were analyzed and characterized by means of FT-IR, XPS, SEMand other means. Simazine, terbuthylazine and cyanazine in the water were tested by SPEcolumn prepared with high performance liquid chromatography (HPLC). Within the range of1.0μg/mL-5.0μg/mL, between of chromatographic peak areas and simazine, terbuthylazineand cyanazine’s concentration were linear. The correlation coefficients (R2) were0.9991,0.9986and0.9961respectively. The relative standard deviation of analysis results were1.19%-3.33%,1.42%-4.99%,4.99%-5.14%respectively. The minimum detection limit were0.7329μg/L,0.9181μg/L,0.6443μg/L respectively. The paper also discussed certain factorswhich influence the extracting efficiency. When flow rate was2mL/min and eluent was2mLacetonitrile and3mL ammoniated methanol, the SPE column had good recovery effect onsimazine, terbuthylazine and cyanazine in the water. The recoveries were77.23%,71.56%and75.04%respectively.