6533b828fe1ef96bd1288fa5

RESEARCH PRODUCT

Evaluation of Thin Film Microextraction for trace elemental analysis of liquid samples using LIBS detection

J. Navarro-gonzálezVincenzo PalleschiStefano LegnaioliL. RipollMontserrat Hidalgo

subject

Analytical chemistryOxide02 engineering and technology01 natural sciencesAnalytical Chemistrylaw.inventionchemistry.chemical_compoundAdsorptionlawDeposition (phase transition)Thin filmGraphene oxideDetection limitLIBSChemistryGraphene010401 analytical chemistryExtraction (chemistry)Trace analysis021001 nanoscience & nanotechnology0104 chemical sciencesLiquid samplesElemental analysisThin Film MicroextractionQuímica Analítica0210 nano-technology

description

An analytical methodology based in the combination of Thin Film Microextraction with Laser-induced Breakdown Spectroscopy (TFME-LIBS) was investigated, for the first time, for detection of Cu, Cr, Ni and Pb in aqueous solutions. In this methodology, the analytes were extracted in a thin film of adsorbent material deposited on a solid support, which was introduced in the sample to analyse. After extraction, the analytes retained in the adsorbent were analysed by LIBS. In order to obtain adsorbent films useful for the microextraction step, two different experimental procedures for film generation, denoted as Drop Casting Deposition and Mould Deposition, were evaluated. In both cases, graphene oxide was used as adsorbent material. The mould deposition procedure was found to produce more homogeneous graphene oxide layers, leading to more uniform distribution of the adsorbed analytes on the graphene oxide surface. Experimental parameters affecting the TFME procedure, such as the adsorbent amount and extraction time, were studied. Under optimum microextraction conditions, the analytical figures of merit of the proposed TFME-LIBS method were evaluated, leading to limits of detection ranging from 41 μg kg−1 and 52 μg kg−1. Method trueness, evaluated from the analysis of a real sample of bottle water, led to recovery values about 70%, indicating the existence of strong matrix effects probably due to the presence of major cations in the bottle water. After 50% dilution of the sample with deionized water, recoveries values improved to 100%–108%. This work was supported by the Spanish Ministry of Economy and Competitiveness [CTQ2016-79991-R], the Regional Government of Valencia (Spain) [PROMETEO/2013/038 and PROMETEO/2018/087]; and the University of Alicante [UAUSTI17-04 and UAUSTI18-04]. L. Ripoll is grateful to the Ministry of Economy and Competitiveness for her PhD fellowship (FPI-MICINN (BES-2012-058759)).

10.1016/j.talanta.2020.121736http://hdl.handle.net/10045/109846