Microwave assisted EDTA extraction-determination of pseudo total contents of distinct trace elements in solid environmental matrices

Abstract

Quantitative determination of metals in environmental matrices became important in the past few decades because of increasing pollutant concentrations in aquatic and terrestrial ecosystems. The extraction phase in the process of determining metals is crucial but very time-consuming. Consequently, new extraction techniques for extractable metals have been developed which probably will substitute conventional procedures in the future. The aim of this study was to improve a closed vessel microwave assisted extraction (MAE) by using EDTA as an exclusive extraction agent (MAE-EDTA) for the determination of pseudo total metal contents in solid environmental samples. For this purpose, a large set of soil and compost samples were analyzed. MAE-EDTA was compared with both closed vessel microwave assisted aqua regia extraction (MAE-AR) and a conventional aqua regia extraction (AR) method for the determination of pseudo total Cd, Cu, Mn, and Pb contents of soil and compost samples. Certified reference materials were used for comparison of recovery rates from different extraction protocols. Metal concentrations in soil and compost extracts were determined by ICP-OES. MAE-AR which was considered as a reference MAE method for further steps of the study, showed the same extraction yields in the determination of pseudo total metal contents of the investigated elements (As, Ba, Be, Cd, Co, Cr, Cu, Mn, Ni, Pb, V, Zn) in soil and compost samples as the conventional AR. MAE-EDTA gave similar values as the reference methods in the determination of Cd, Cu, and Pb amounts in soil samples and Cd, Mn, and Pb amounts in compost samples. The recovery rates ranged between 89.0-117.1% for soil samples and 93.5-104.0% for compost samples. MAE-EDTA provides fast processing of the samples that is less than one hour, including time for cooling of the samples. Apart from significantly less processing time, minimal consumption of sample and reagent chemicals is a strategic characteristic of MAE-EDTA procedure which has advantages including accuracy and reduction of contamination. The drawback of MAE-EDTA was that the optimized conditions for the metals Cd, Cu, Mn and Pb may not be generally applicable for the other metals. Therefore, the analytical parameters available in MAE-EDTA should be further investigated for the metals of interest.