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作 者:李改花 刘爽[1] 罗宝晶 LI Gaihua;LIU Shuang;LUO Baojing(Tangshan Key Laboratory of Green Specialty Chemicals,Department of Chemistry,Tangshan Normal University,Tangshan 063000,China)
机构地区:[1]唐山师范学院化学系,唐山市绿色专用化学品重点实验室,唐山063000
出 处:《理化检验(化学分册)》2023年第7期776-782,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:唐山师范学院科学研究基金项目(2020A01)。
摘 要:采用均匀沉淀法制备纳米SnS/多壁碳纳米管(MWCNTs)复合物,利用场发射扫描电子显微镜(SEM)、X射线粉末衍射仪(XRD)和热重分析仪(TGA)对其形貌和组成进行表征。将纳米SnS/MWCNTs复合物10 mg超声分散在1.0 mL 5%(体积分数)全氟化树脂溶液中,分取8.0μL滴涂于处理好的玻碳电极(GCE)表面,得到修饰电极(纳米SnS/MWCNTs/GCE)。以纳米SnS/MWCNTs/GCE为工作电极,铂丝电极为对电极,饱和甘汞电极为参比电极,采用循环伏安法(CV)、电化学阻抗谱法(EIS)和差分脉冲伏安法(DPV)对纳米SnS/MWCNTs/GCE电化学性能进行考察,研究了2,4-二氯苯酚(2,4-DCP)在纳米SnS/MWCNTs/GCE上的电化学行为。结果表明:在pH 7.0的磷酸盐缓冲溶液中,纳米SnS/MWCNTs/GCE对2,4-DCP有明显的电催化作用和较高的选择性;2,4-DCP的浓度在0.05~3.00μmol·L^(-1)内与DPV响应的氧化峰电流呈线性关系,检出限(3S/N)为2.3×10^(-8)mol·L^(-1);按照标准加入法对水样进行回收试验,2,4-DCP回收率为92.0%~101%。Nano-SnS/multi-walled carbon nanotubes(MWCNTs) composite was prepared through homogeneous precipitation method,and the morphology and constitution were characterized by field emission scanning electron microscopy(SEM),X-ray powder diffractometer(XRD) and thermal gravimetric analyzer(TGA).Nano-SnS/MWCNTs composite(10 mg) was dispersed in 1.0 mL of 5%(volume fraction) perfluorinated resin solution by ultrasonic,and the modified electrode was obtained by dripping 8.0 μL of aliquot onto the surface of treated glassy carbon electrode(GCE),which was denoted as nano-SnS/MWCNTs/GCE.The electrochemical property of nano-SnS/MWCNTs/GCE was investigated by cyclic voltammetry(CV),electrochemical impedance spectroscopy(EIS) and differential pulse voltammetry(DPV) using nano-SnS/MWCNTs/GCE as working electrode,platinum wire electrode as counter electrode,and saturated calomel electrode as reference electrode,and the electrochemical behavior of 2,4-dichlorophenol(2,4-DCP) on nano-SnS/MWCNTs/GCE was studied.As shown by the results,nano-SnS/MWCNTs/GCE had obvious electrocatalytic effect and high selectivity for 2,4-DCP in phosphate buffer solution at pH 7.0.Linear relationship between the concentration of 2,4-DCP and the oxidation peak current by DPV response was kept in the range of 0.05-3.00 μmol·L^(-1),with detection limit(3S/N) of 2.3×10^(-8)mol·L^(-1).Test for recovery was made on the water sample by standard addition method,giving results in the range of 92.0%-101% for 2,4-DCP.
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