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用于伏安法检测亚纳摩尔水平甲基对硫磷的含碳和氧化铁(III)的氧化锆纳米复合材料

Zirconia nanocomposites with carbon and iron(iii) oxide for voltammetric detection of sub-nanomolar levels of methyl parathion.

作者信息

Gannavarapu Krishna Prasad, Ganesh V, Dandamudi Rajesh Babu

机构信息

Department of Chemistry, Sri Sathya Sai Institute of Higher Learning Prasanthinilayam Campus, Puttaparthi Anantapur Dist. Andhra Pradesh 515134 India

Electrodics and Electrocatalysis Division, CSIR-Central Electrochemical Research Institute Karaikudi Tamil Nadu 630001 India.

出版信息

Nanoscale Adv. 2019 Oct 29;1(12):4947-4954. doi: 10.1039/c9na00589g. eCollection 2019 Dec 3.

Abstract

This study reports the synthesis of zirconia nanoparticles loaded on various carbon substrates, namely, reduced graphene oxide (Zr-r-GO), carbon nanotubes (Zr-CNT), and activated carbon (Zr-AC). In addition, a composite of zirconia-iron mixed oxide loaded on activated carbon (FeZr-AC) was also synthesized. The materials were characterized using SEM-EDX, HRTEM, FTIR, Raman spectroscopy, TGA and XRD. The FeZr-AC sample was found to have a nanorod like morphology. The samples were evaluated for their sensing potential towards methyl parathion (MP) using differential pulse voltammetry in a range of 0.0 V to -0.9 V ( Ag/AgCl) by drop casting on a glassy carbon electrode (GCE). All the modified GCEs best operated at a working potential of 0.4-0.9 V Ag/AgCl/Cl. FeZr-AC was found have the best limit of detection followed by Zr-AC, Zr-CNT and Zr-r-GO with their detection limits being 1.7 × 10 M, 17.2 ×10 M, 243.3 × 10 M and 534.0 × 10 M respectively. These materials were then used to detect MP in spiked sewage samples and showed good recoveries.

摘要

本研究报道了负载在各种碳基底上的氧化锆纳米颗粒的合成,即还原氧化石墨烯(Zr-r-GO)、碳纳米管(Zr-CNT)和活性炭(Zr-AC)。此外,还合成了负载在活性炭上的氧化锆-铁混合氧化物复合材料(FeZr-AC)。使用扫描电子显微镜-能谱仪(SEM-EDX)、高分辨率透射电子显微镜(HRTEM)、傅里叶变换红外光谱仪(FTIR)、拉曼光谱仪、热重分析仪(TGA)和X射线衍射仪(XRD)对这些材料进行了表征。发现FeZr-AC样品具有纳米棒状形态。通过滴铸在玻碳电极(GCE)上,使用差分脉冲伏安法在0.0 V至-0.9 V(Ag/AgCl)范围内评估了这些样品对甲基对硫磷(MP)的传感潜力。所有修饰的玻碳电极在0.4 - 0.9 V Ag/AgCl/Cl的工作电位下表现最佳。发现FeZr-AC的检测限最佳,其次是Zr-AC、Zr-CNT和Zr-r-GO,它们的检测限分别为1.7×10⁻⁹ M、17.2×10⁻⁹ M、243.3×10⁻⁹ M和534.0×10⁻⁹ M。然后使用这些材料检测加标污水样品中的MP,并显示出良好的回收率。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/cf37/9419288/997a49761189/c9na00589g-f1.jpg

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