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采用改进的Hummers法和硼氢化钠还原法制备Pd/石墨烯催化剂,并采用XRD、SEM、XPS、TEM等技术对其进行表征.将该催化剂修饰于玻碳电极表面,制备出Pd/石墨烯/玻碳电极,使用循环伏安法研究了检测4-氯酚的最佳工作条件.研究结果表明,所得石墨烯表面平整光滑,以零价态存在的Pd纳米颗粒均匀分散到石墨烯上,平均粒径为(6.5±0.05)nm.检测4-氯酚的最佳支持电解质为0.1 mol·L-1、p H 6.8的磷酸-磷酸钠缓冲溶液(PBS),峰电流与扫描速率的平方根呈良好的线性关系(R2=0.992),该电极的线性范围为1~100μmol·L-1(R2=0.967),检测限为0.57μmol·L-1(S/N=3),且具有良好的重现性和稳定性.本文所研制的Pd/石墨烯/玻碳电极具有较高的催化活性,提供了一种简便快捷、重现性好的检测4-氯酚的方法.
Pd / graphene catalysts were prepared by the modified Hummers method and sodium borohydride reduction method, and the catalysts were characterized by XRD, SEM, XPS, TEM etc. The catalyst was modified on the surface of glassy carbon electrode to prepare Pd / graphene / Glassy carbon electrode, the best working conditions for the determination of 4-chlorophenol were studied by cyclic voltammetry.The results show that the surface of graphene obtained is flat and smooth, the Pd nanoparticles existing in zero valence state are uniformly dispersed on the graphene, The average particle size was (6.5 ± 0.05) nm. The best support electrolyte for 4-chlorophenol was 0.1 mol·L-1, PBS, the peak current and the square root of the scan rate (R2 = 0.992). The linear range of the electrode was 1 ~ 100μmol·L-1 (R2 = 0.967), the detection limit was 0.57μmol·L-1 (S / N = 3) The reproducibility and stability of Pd / graphene / glassy carbon electrode developed in this paper have high catalytic activity and provide a simple, rapid and reproducible method for the detection of 4-chlorophenol.