Elsevier

Chemical Geology

Volume 124, Issues 1–2, 25 July 1995, Pages 109-123
Chemical Geology

Sequential extraction of soils for multielement analysis by ICP-AES

https://doi.org/10.1016/0009-2541(95)00029-LGet rights and content

Abstract

Realistic environmental interpretation of soil contamination depends on an understanding of how metals are bound to the various phases in the soil. A five-step sequential chemical extraction scheme, originally designed for sediment analysis by flame atomic adsorption spectroscopy (FAAS), has been developed for the multielement analysis of soils by inductively coupled plasma-atomic emission spectrometry (ICP-AES). Each of the chemical fractions is operationally defined as follows: (1) exchangeable; (2) bound to carbonates or specifically adsorbed; (3) bound to FeMn-oxides; (4) bound to organic matter and sulphides; and (5) residual. The number of elements determined by ICP-AES has been extended to fifteen (Be, Ca, Co, Cr, Cu, Fe, K, Li, Mn, Ni, P, Pb, Ti, V, Zn), which include most of the major elements, thereby increasing the potential of the sequential extraction method by enabling broader studies of geochemical associations in soils. The precision was estimated to be ∼ 5% (2σ) for each extraction step. The overall recovery rates of international reference materials were between 85 and 110% for most elements, with an average of 92%. There is good agreement between the results for the international reference material (USGS MAG-1) in each extraction step and published values. A wide range of soil reference materials, including SO-1-SO-4 and BCR141-BCR143, were also analysed for future comparison. The application of the method to soils contaminated by past mining and smelting activities showed distinctive partitioning patterns of heavy metals from the two sources. The multielement measurements gave useful information to assist in the interpretation of the possible geochemical forms and sources of the trace elements in soils.

References (38)

  • T.E. Clevenger et al.

    Lead speciation of particles on air filters collected in the vicinity of a lead smelter

    Environ. Sci. Technol.

    (1991)
  • P. Colbourn et al.

    Lead pollution in agricultural soils

    J. Soil Sci.

    (1978)
  • J. Cotter-Howells et al.

    Sources and pathways of environmental lead to children in a Derbyshire mining village

    Environ. Geochem. Health

    (1991)
  • U. Förstner

    Chemical forms and reactivities of metals in sediments

  • R.L. Foster et al.

    X-ray diffractometry examination of air filters for compounds emitted by lead smelting operations

    Environ. Sci. Technol.

    (1980)
  • R.M. Harrison et al.

    Chemical association of lead, cadmium, copper, and zinc in street dust and roadside soil

    Environ. Sci. Technol.

    (1981)
  • M.G. Hickey et al.

    Chemical partitioning of cadmium, copper, nickel, and zinc in soils and sediments containing high levels of heavy metals

    J. Environ. Qual.

    (1984)
  • E.A. Jenne

    Trace element sorption by sediments and soils — site and processes

  • J.M. Jouanneau et al.

    Critical analysis of sequential extractions through the study of several attack constituent residues

    Environ. Technol. Lett.

    (1983)
  • Cited by (285)

    • Assessment of heavy metal stability in biochar-treated soil

      2023, Biochar Application in Soil to Immobilize Heavy Metals: Fundamentals and Case Studies
    • Immobilization and recycling of contaminated marine sediments in cement-based materials incorporating iron-biochar composites

      2022, Journal of Hazardous Materials
      Citation 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).

    View all citing articles on Scopus
    View full text