Layered double hydroxides: a novel nano-sorbent for solid-phase extraction.

The nickel-aluminum layered double hydroxide (Ni-Al LDH) was synthesized by a simple co-precipitation method with controlled pH and followed by hydrothermal treatment. The obtained nano-structured inorganic material was employed, for the first time, as a new solid-phase extraction (SPE) sorbent for the extraction and pre-concentration of trace levels of fluoride ions from aqueous solutions. An indirect method was used for monitoring of extracted fluoride ions. The method is based on the quenching effect of extracted fluoride ions upon the fluorescence intensity of Al-oxine complex via the forming of AlF(6)(3-), which was determined spectrofluorometrically at λ(em)=510 nm with excitation at λ(ex)=404 nm. The effect of several parameters such as type of interlayer anion in Ni-Al LDH structure, pH, sample flow rate, elution conditions, amount of nano-sorbent, sample volume and co-existing ions on the extraction efficiency of the analyte were investigated. The results showed that fluoride ions could be retained on the Ni-Al (NO(3)(-)) LDH at pH 6.0 and stripped by 1.2 mL of 3.0 mol L(-1) NaOH. In the optimum experimental conditions, the limit of detection (3s) and enrichment factor were 9.0 ng mL(-1) and 50, respectively. The optimized method was successfully applied to the determination of fluoride concentration in various water samples. The results obtained from the proposed method were successfully compared with those provided by standard SPADNS method.