Zirconia hollow fiber: preparation, characterization, and microextraction application.
Zirconia hollow fiber: preparation, characterization, and microextraction application.
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DOI：
10.1021/ac070449b
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发表时间：
2007-06
影响因子：
7.4
通讯作者：
L. Xu;Hian Kee Lee
中科院分区：
文献类型：
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作者：
L. Xu;Hian Kee Lee
首次采用模板法结合溶胶-凝胶法成功地制备了大孔氧化锆中空纤维膜。采用聚丙烯中空纤维作为模板。制备过程包括将模板反复浸渍在合适的氧化锆溶胶前驱体中，并煅烧以烧掉模板，从而制备氧化锆中空纤维。所得中空纤维膜在形态学方面与其模板几乎相同，表现出中空芯结构。除此之外，它还具有与其模板不同的双峰多孔子结构、窄分布的纳米骨架孔和均匀的纹理孔或通孔。壁厚和亚结构可以通过合成条件和后热处理方便地控制。此外，如此制备的氧化锆中空纤维被应用于神经毒剂降解产物的微萃取和浓缩，然后进行液相色谱-质谱分析。由于氧化锆纤维作为单独的装置存在并且可直接用于提取，因此处理比例如需要涂覆在杆上用于提取过程的粉末形式的吸附剂更方便。此外，它易于制备，并且在这个意义上上级单片材料。以有机磷神经毒剂梭曼的降解产物甲基膦酸频哪醇酯为模型分析物。氧化锆中空纤维被证明是一种高选择性的吸附剂，具有高灵敏度的含膦酸化合物。检测限低至0.07 ng/mL（0.39 nM）。
A zirconia hollow fiber membrane in the macrorange was for the first time successfully synthesized via a template method coupled with a sol-gel process. A polypropylene hollow fiber was employed as the template. The preparation procedure includes repeated impregnation of the template in the proper zirconia sol precursor, and calcination to burn off the template, producing the zirconia hollow fiber. The resulting hollow fiber membrane is almost identical to its template in terms of morphology, exhibiting a hollow core structure. In addition to that, it has a bimodal porous substructure that is different from its template, narrowly distributed nanoskeleton pores, and uniform textural pores or throughpores. The wall thickness and substructures can be conveniently controlled by the synthetic conditions and postheat treatment. Moreover, the thus-prepared zirconia hollow fiber was applied for the microextraction and concentration of a nerve agent degradation product followed by liquid chromatography-mass spectrometric analysis. Since the zirconia fiber exists as an individual device and is directly usable for extracting, handling is more convenient than, for example, an adsorbent in powder form that needs to be coated on a rod for the extraction process. In addition, it is easily prepared and is superior to the monolithic material in this sense. Pinacolyl methylphosphonic acid, one degradation product of organophosphorus nerve agent (soman), was used as the model analyte. Zirconia hollow fiber was demonstrated to be a highly selective adsorbent for the phosphonic acid-containing compounds with high sensitivity. Limit of detection was as low as 0.07 ng/mL (0.39 nM).