Development of a Rapid and Simple Digestion Method of Freshwater Sediments for As, Cd, Cr, Cu, Pb, Fe, and Zn Determination by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES): An Evaluation of Dilute Nitric Acid

Abstract

ABSTRACT In this study, a simple and rapid methodology based on the hot-plate digestion method using dilute nitric acid solution was used to extract trace metals (such as As, Cd, Cr, Cu, Pb, Fe, and Zn) from freshwater sediments. The concentrations of the elements were determined using inductively coupled plasma-optical emission spectrometry (ICP-OES). The factors (temperature, nitric acid concentration, and volume) affecting the digestion method were optimized using one-factor-at-a-time (OFAT) or univariate methodology, and the optimization process was carried out using freshwater sediment certified reference material (CRM015). The optimal conditions for temperature, nitric acid concentration, and time in the method were 180°C, 10 mL of 5 mol L−1 HNO3, and 45 min, respectively. Under optimum conditions, the limit of detection (LOD) ranged between 0.02 and 0.08 µg L−1 and the limit of quantification (LOQ) ranged from 0.07 and 0.27 µg L−1. In addition, the method detection limits (MDLs) and method quantification limits (MQLs) were 0.10–0.17 and 0.30−0.57 µg g−1, respectively. The overall accuracy of the method determined by recovery of the trace elements in the CRMs ranged from 98 to 111% with the precision ranging from 1.4 to 5.8%. The method was successfully applied for the determination of target metals from real freshwater sediment samples.