A single step technique for preparation of porous solid phase microextraction fibers by electrochemically co-deposited silica based sol–gel/Cu nanocomposite

In this study, electrochemically co-deposited 3-trimethoxysilyl propyl methacrylate (3TMSPMA)/Cu nanocomposite is introduced as a novel and single-step technique for preparation of efficient and unbreakable solid phase microextraction (SPME) fibers; having strong interaction between the substrate and the coating. The applicability of prepared nanocomposite films was evaluated through extraction of some aromatic pollutants as model compounds from the headspace of aqueous samples in combination with gas chromatography–mass spectrometry (GC–MS). Different parameters affecting the structure and composition of the deposited films including applied potential, electrodeposition time, and precursor concentration; and the parameters affecting extraction efficiency such as extraction temperature, extraction time, and salt content were investigated. The results showed that morphology and grain size of the films are strongly affected by the ratio between the sol–gel precursor and Cu2+ ions. Furthermore, potential of deposition influences the composition of films as it controls the kinetics of sol–gel/Cu co-deposition. Finally, characterization of the deposited films was accomplished by scanning electron microscopy (SEM) and thermogravimetric analysis (TGA).

► A novel technique for preparation of solid phase microextraction fibers was proposed.
► It does not need to activate the surface of the substrate before coating.
► Strong interaction between coating and substrate is produced.
► The coating has porous structure.
► This technique is an easy and inexpensive technique to prepare unbreakable fibers.