Cold finger with semi closed reflux system for sample preparation aiming at Al, Ca, Cr, Cu, Fe, K, Mg, Mn, Ni, V and Zn determination in Drinking Water Treatment Sludge by MIP OES

This study presents method development and optimization, based on statistical approaches, of an alternative sample preparation methodology for Drinking Water Treatment Sludge, through decomposition in semi closed system with cold finger, aiming at the determination of Al, Ca, Cr, Cu, Fe, K, Mg, Mn, Ni, V and Zn by microwave induced plasma optical emission spectrometry. This system was employed to decompose three different Drinking Water Treatment Sludge samples, from three different treatment plants. The compromise conditions were 250 mg of dried sample, 5 mL of HNO₃, 1 mL of H₂SO₄ and heating at 225 °C for 150 min. After the digestion, 1% of cesium and lanthanum chloride buffer solution was added to all samples and standard solutions. The accuracy of the proposed sample preparation method was evaluated by analyzing a sediment certified reference material (CRM NIST 1646a) as well as the spike recovery technique. The recoveries ranged from 83% to 119% for all elements, and the found concentrations for the CRM agreed with the respective certified values, at 95% confidence level. The correlation coefficients for all investigated elements were higher than 0.999. The method LOQ values were adequate and complied with the Drinking Water Treatment Sludge regulation avaliable, ranging from 0.3 (V) and 32 (Zn) μg L^-1, or 0.1 (V) to 13 (Zn) mg kg^-1. The digestion procedure in acidic medium showed suitable to measure the analytes in the investigated matrix by microwave induced plasma optical emission spectrometry.