Abstract

Carbon xerogels (CXs) were synthesized by polycondensation of resorcinol and formaldehyde, followed by thermal annealing, and subjected to hydrothermal oxidation. Solid-phase extraction (SPE) cartridges were filled with CXs and tested for extraction of metaflumizone and other seven environmental micropollutants (acetamiprid, atrazine, isoproturon, methiocarb, carbamazepine, diclofenac, and perfluorooctanesulfonic acid) before chromatographic analysis. The recoveries obtained with the pristine CX were low for most analytes, except for metaflumizone (69 ± 5%). Moreover, it was concluded that the adsorption/desorption process of the micropollutants performed better on CXs with a less acidic surface (i.e., pristine CX). Thus, cartridges were prepared with pristine CX and multi-walled carbon nanotubes (MWCNTs) in a multi-layer configuration. This reusable cartridge was able to simultaneously extract the eight micropollutants and was used to validate an analytical methodology based on SPE followed by ultra-high performance liquid chromatography-tandem mass spectrometry. A widespread occurrence of 6/8 target compounds was observed in surface water collected in rivers supplying three drinking water treatment plants and in the resulting drinking water at the endpoint of each distribution system. Therefore, the first study employing CXs and MWCNTs as sorbent in multi-layer SPE cartridges is herein reported as a proof of concept for determination of multi-class water micropollutants.

Highlights

  • Carbon xerogels (CXs) were synthesized by polycondensation of resorcinol and formaldehyde, followed by thermal annealing, and subjected to hydrothermal oxidation

  • Since organic micropollutants (OMPs) are typically found at residual concentrations in the environment, it is important to employ an accurate and precise preconcentration step prior to the analysis by using a sensitive and reproducible analytical technique, such as ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS)

  • The definitive screening design (DSD), which involved 14 randomized experiments with 5 factors (mass of sorbent material, sample volume, sample pH, type of solvent and solvent volume) and 3 levels (− 1, 0 and 1), was applied in a first stage aiming for the determination of the main parameters affecting the recovery efficiency of the 8 target OMPs

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Summary

Introduction

Carbon xerogels (CXs) were synthesized by polycondensation of resorcinol and formaldehyde, followed by thermal annealing, and subjected to hydrothermal oxidation. Cartridges were prepared with pristine CX and multi-walled carbon nanotubes (MWCNTs) in a multi-layer configuration This reusable cartridge was able to simultaneously extract the eight micropollutants and was used to validate an analytical methodology based on SPE followed by ultra-high performance liquid chromatographytandem mass spectrometry. The first study employing CXs and MWCNTs as sorbent in multi-layer SPE cartridges is reported as a proof of concept for determination of multi-class water micropollutants. In the field of analytical chemistry, only two studies were found in the literature for the analysis of pollutants by using CXs in SPE: (i) one to determine the effectiveness of an oxidized CX material as sorbent in SPE to preconcentrate lead from tap water s­ amples[32]; and (ii) another to extract aryloxyphenoxypropionate herbicides from aquatic environmental samples by micro-SPE31. Studies focused on the application of CXs as SPE adsorbent for extraction of other ­PSs2 or CECs listed in the Watch List of the EU D­ ecisions[3,4,5] were not found

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