Time-saving application for sequential extraction of heavy metals by optimized BCR method and lixiviation from untreated sewage sludge

Abstract

This article describes an improvement in the modified BCR three-step sequential extraction procedure employed for heavy metals (Cd, Cr, Cu, Ni, Pb and Zn) in untreated domestic waste-water sewage sludge collected from different cities in Pakistan.The BCR sequential extraction protocol requires 16 h for each step, whereas in the present work optimum recoveries of all heavy metals were attained in 10 h/step. The validity of the proposed BCR sequential extraction procedure was checked using certified reference material (BCR 483). Various parameters such as time interval (2–16 h) and sample mass (0.2–1.0 g) were studied to achieve optimum recovery of the heavy metals studied. The extracted analytes were determined by atomic absorption spectrometry. The optimum recovery of heavy metals from the certified reference material and from experimental samples was achieved at a sample mass of 0.4 g, while the time required for extraction on a mechanical shaker at 30 rpm was found to be 26–32 h. The sequence of easily available (acid-exchangeable) heavy metals was determined as Cd<Zn<Ni<Cr<Pb<Cu. With the exception of Cd the dominant fractions of the heavy metals were associated with organic matter, while 31.0 and 47.8% of Cd was present in acid-soluble and reducible forms, respectively. A lixiviation test (DIN 38414-S4) was used to evaluate the leaching of heavy metals from the domestic waste-water sewage sludge used for agricultural purposes.