Sequential extraction of soils for multielement analysis by ICP-AES
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2022, Journal of Hazardous MaterialsCitation Excerpt :The pore size distribution of the S/S products was determined by mercury intrusion porosimetry (MIP, AUTOPORE IV 9500). Toxicity characteristic leaching procedure (TCLP) (US EPA, 1992): 0.1 M glacial acetic acid (pH 2.88 ± 0.05) was used at a liquid to solid ratio of 20 mL/g by an end-to-end rotator at 30 rpm for 18 h. Sequential extraction procedure (SEP): The extraction was carried out in 50 mL polyethylene centrifuged tubes with 1 g solid samples according to the literatures with minor modifications (Li et al., 1995; Wang et al., 2020). The fractions determined were: exchangeable (F1) (8 mL 1 M MgCl2 at pH 7.0 for 1 h), carbonates or acid soluble (F2) (8 mL 1 M NaOAc at pH 5 for 5 h), reducible or Fe-Mn oxide bounded (F3) (20 mL 0.04 M NH2OH·HCl in 25% (V/V) HOAc at 96 ± 3 °C for 6 h), oxidizable (F4) (3 mL 0.02 M HNO3 + 5 mL 30% H2O2 at pH 2 and 85 ± 2 °C for 2 h, add 3 mL 30% H2O2 for 3 h, cool down, add 5 mL 3.2 M NH4OAc in 20% (v/v) HNO3 for 0.5 h), and residual fraction (F5) (use HClO4 mL and HNO3 4 mL for total digestion).