In-site and solvent-free exfoliation of porous graphene oxide from pencil lead fiber for solid-phase microextraction of cadmium ion before GF-AAS determination.

Graphene oxide (GO)-functionalized pencil lead fiber was prepared for the first time by in situ oxidation and exfoliation of graphite contained in pencil lead fiber to porous graphene oxide structure via a one-step solvent-free dielectric barrier discharge (DBD) microplasma treatment. This new fiber was demonstrated as a highly efficient and low-cost solid-phase microextraction (SPME) fiber for the determination of toxic metal ions. The fiber extraction performance was evaluated by using cadmium as a model analyte in a direct immersing SPME mode. Unlike most commercially available and other lab-built fibers, the preparation of the graphene oxidized pencil lead fiber is environmentally friendly, low cost, and non-toxic without using any organic solvents. The fiber is robust due to its coating-free configuration. Furthermore, high extraction efficiency and high sensitivity for cadmium can be obtained due to the abundant oxygen-containing functional groups on the surface of the novel fiber. After extraction, the cadmium adsorbed on the fiber was desorbed to 150-µL solution. Graphite furnace atomic absorption spectrometry (GF-AAS) with low sample consumption was used to determine cadmium. The calibration curve for cadmium ions was linear in a range 0.04-0.26 µg L-1 with a detection limit of 0.005 µg L-1. A relative standard deviation (RSD, n = 5) of 2.1% was obtained at 0.1 µg L-1 of cadmium. The sensitivity enhancement factor (EF) value of the proposed SPME method was 25. The SPME fiber was successfully applied to determine cadmium in tap water, river water, and pond water with spike recoveries ranging from 94 to 105%. Pipe network water samples were also analyzed to evaluate the cadmium release to drinking water due to the corrosion of tubes.