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采用水热氧化法制备镍钛合金(Ni Ti)固相微萃取纤维。实验结果表明,在80℃的H2O2溶液中,直接氧化Ni Ti纤维基体可在其表面原位生长纳米多孔氧化镍/氧化钛复合涂层,其中氧化镍含量显著高于氧化钛含量。与高效液相色谱-紫外检测器(HPLC-UV)检测技术联用,考察了所制备Ni Ti纤维对典型芳香族化合物的萃取性能。结果表明,富Ni复合氧化物涂层对多环芳烃(PAHs)表现出良好的萃取选择性。在优化实验条件下,方法的线性范围为0.1~400.0 ng/m L,相关系数大于0.999,PAHs的检出限为0.026~0.056 ng/m L。对于50 ng/m L加标水样,单支Ni Ti纤维日内和日间测量的相对标准偏差(RSDs)分别为4.8%~6.2%和5.4%~6.5%(n=5),使用5支不同批纤维测量的RSDs为6.4%~8.4%。本方法适用于环境水样中PAHs的富集和测定,相对回收率为89.9%~108.5%,RSDs<8.1%。而且,Ni Ti纤维机械强度高,化学稳定性好,制备过程精密可控。
NiTi solid phase microextraction fibers were prepared by hydrothermal method. The experimental results show that the direct oxidation of Ni Ti fiber substrate can grow nanoporous nickel oxide / titanium oxide composite coating in situ on the surface of the substrate at 80 ℃ in H2O2 solution, in which the content of nickel oxide is significantly higher than that of titanium oxide. In combination with the HPLC-UV detector, the extraction performance of typical aromatic compounds of Ni Ti fibers was investigated. The results show that Ni-rich composite oxide coatings exhibit good extraction selectivity for PAHs. Under the optimized experimental conditions, the linear range of the method was 0.1-400.0 ng / mL, the correlation coefficient was greater than 0.999, and the detection limit of PAHs was 0.026-0.05 6 ng / mL. For 50 ng / m L spiked water samples, the relative standard deviations (RSDs) of single Ni Ti fibers were 4.8% -6.2% and 5.4% -6.5%, respectively (n = 5) The RSDs of different batches of fibers measured 6.4% ~ 8.4%. The method is suitable for the enrichment and determination of PAHs in environmental water samples with relative recoveries of 89.9% -108.5% and RSDs <8.1%. Moreover, Ni Ti fiber high mechanical strength, chemical stability, the preparation process is precisely controlled.