Abstract

In this paper, Fe3O4 nanoparticles (Fe3O4 NPs) grafted carboxyl groups of multiwalled carbon nanotubes with cationic polyelectrolyte poly (dimethyldiallylammonium chloride) (PDDA) (MWCNTs-COO−/PDDA@Fe3O4), are successfully synthesized and used for the extraction of six kinds of major toxic polychorinated biphenyls (PCBs) from a large volume of water solution. The hydrophilicity of the PDDA cage can enhance the dispersibility of sorbents in water samples, and the superparamagnetism of the Fe3O4 NPs facilitate magnetic separation which directly led to the simplification of the extraction procedure. With the magnetic solid-phase extraction (MSPE) technique based on the MWCNTs-COO−/PDDA@Fe3O4 sorbents, it requires only 30 min to extract trace levels of PCBs from 500 mL water samples. When the eluate condensed to 1.0 mL, concentration factors for PCBs became over 500. The spiked recoveries of several real water samples for PCBs were in the range of 73.3–98.9% with relative standard deviations varying from 3.8% to 9.4%, reflecting good accuracy of the method. Therefore, preconcentration of trace level of PCBs by using this MWCNTs-COO−/PDDA@Fe3O4 sorbent, which are stable for multiple reuses, from water solution can be performed.

Highlights

  • Polychlorinated biphenyls (PCBs), a class of chlorinated aromatic hydrocarbon chemicals that are known as a part of the persistent organic pollutants (POPs), are highly toxic and resistant to degradation in the environment [1]

  • G−1 is enough for magnetic separation from solution with a magnet [22]. These imply that Multi-walled carbon nanotubes (MWCNTs)-COO−/PDDA@Fe3O4 sorbents can be dispersed into water solution readily and the magnetic sorbent loaded with analytes can be isolated from the matrix conveniently by using an external magnet when necessary

  • From the XRD pattern of MWCNTs-COO−/PDDA@Fe3O4 analysis, the main characteristic peaks of Fe3O4 and MWCNTs located at 26°, 30.1°, 35.4°, 43.3°, 57.3°and 62.8°, indicating that the product is composed of two phases: Fe3O4 and MWCNTs

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Summary

Introduction

Polychlorinated biphenyls (PCBs), a class of chlorinated aromatic hydrocarbon chemicals that are known as a part of the persistent organic pollutants (POPs), are highly toxic and resistant to degradation in the environment [1]. Many researchers have studied the modification of CNTs by introducing special functional groups on its surface in order to enhance its adsorption capacity for organic aromatic compounds and improve its dispersion property in aqueous solutions [13,14,15]. These nanosized sorbents have great solubility and high extraction efficiency. Our study aims to develop a novel magnetic nanoparticle of MWCNTs-COO−/PDDA@Fe3O4 as stationary phase of SPE and their potential applications in the enrichment of PCBs from environmental water samples.

Particle Size and Morphology
IR Spectra
Magnetic Properties
Magnetic Separation and Adsorption Equilibrium Time
Effect of the Solution pH
Effect of Elution Solvent
Volume of Elution Solvent
Effect of Desorption Flow Rate
Reusability of the Sorbents
Method Validation
Determination of PCBs in Environmental Water Samples
Chemicals and Materials
Preparation of Fe3O4 Nanospheres
Material Characterization
Magnetic SPE Procedure
GC-MS Analysis
Real Sample Preparation
Conclusions
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