随着针对过氧化物研究的深入，其应用范围遍布生产生活以及科学研究的各个领域。其中，过一硫酸盐（PMS）作为具有较高安全浓度的消毒剂以及产生硫酸根自由基的前驱体化合物，在食品安全、畜牧以及地下水修复等方向有普遍的应用，已经成为了不同科研领域的研究热点。所以开发PMS快速分析方法对于推动过氧化物研究进一步的发展有着重要意义。

本研究基于胶束微环境中的过一硫酸盐和铽配体的化学发光现象，提出了一种快速灵敏的流动注射化学发光法检测PMS方法，其中合适的有机配体以及表面活性剂形成的胶束微环境可以为体系创造最优的能量转移途径和微环境，提高方法的灵敏度；并将该方法应用于不同样品中的PMS测定和过一硫酸盐分解过程中的动力学研究。在最优的实验条件下，过一硫酸盐的线性范围从4.0×10^-6 mol/L到 2.0×10^-4 mol/L（r=0.9997）,检出限为5.0×10^-7 mol/L（S/N=3），同时对于连续测定9次1.0×10^-5 mol/L的过一硫酸盐来说，其相对标准偏差为2.4%；所建立的方法抗干扰性和选择性较强，水环境种所存在的常见离子都不会影响该方法的检测性能。该方法已成功用于卫可消毒粉、自来水和游泳池水中样品的PMS测定，回收率为94.8％-104.8％。该方法基于检测瞬时化学发光现象，而且在检测前不需要反应过程或者分离步骤，所以可以实现PMS的快速检测，分析频率可以达到每分钟五次。该快速化学发光方法也已成功地用于研究不同碳材料（碳纳米管，碳纳米纤维，活性炭和氧化石墨烯）催化体系中的过一硫酸盐的分解过程研究，其反应动力学过程可以用一级反应动力学（r> 0.9305）方程很好拟合。自由基淬灭实验和电子自旋共振谱证明，化学发光现象是由于单线态氧的生成所引发，在反应过程中，羟基自由基和硫酸根自由基可能对单线态氧的生成起重要的作用。根据不同介质中的荧光光谱和化学发光光谱的对比结果，表明三价铽是反应过程中重要的发光体。利用检测灵敏度较高的流动注射化学发光技术建立PMS的快速分析方法为拓展和优化现有过氧化物分析技术提供有效支撑。

With the deepening of the research on peroxide, its application scope covers all fields of production, life and scientific research. Among them, persulfate (PMS) as a disinfectant with a higher safe concentration and a precursor compound that generates sulfate radicals, its own research has become a research hotspot in different scientific fields; involving food safety, animal husbandry and remediation of groundwater and other directions. Therefore, the development of PMS rapid analysis method is of great significance for the further development of peroxide research.

Based on the chemiluminescence (CL) phenomena of peroxymonosulfate (PMS) and Tb(III) enhanced by its ligand in micelle microenvironment, a fast and sensitive flow injection CL method for PMS detection was proposed and applied to the analysis of different samples and PMS decomposition. Under the optimized conditions, a linear range was obtained from 4.0×10^-6 mol/L to 2.0×10^-4 mol/L with a high correlation coefficient (r=0.9997), detection limit of 5.0×10^-7 mol/L (S/N=3) and relative standard deviation of 2.4 % for 1.0×10^-5 mol/L PMS (n=9). The established method has strong anti-interference and selectivity, and the common ions present in the water environment species will not affect the detection performance of the method. It was successfully applied to the determination of PMS in Virkon powder, tap water and swimming pool water samples with satisfactory recoveries from 94.8% to 104.8%. In particular, the analytical frequency could be as fast as 5 samples per minute because there is no reaction step before analysis and the CL phenomena are instantaneous. Therefore, this CL method has also been successfully applied to investigate the PMS decomposition profiles in carbon material (carbon nanotubes, carbon nanofibers, activated carbon and graphene oxide) catalysis systems, which followed pseudo-first-order kinetics with good correlation coefficients (r>0.9305). Quenching experiments and electron spin resonance spectra verified that the CL phenomena were due to the formation of singlet oxygen, and hydroxyl and sulfate radicals might be important to the generation for singlet oxygen. Tb(III) is the luminescent emitter according to the characteristics emission bands of the fluorescence and CL spectra in different media.