Should acid ammonium oxalate replace hydroxylammonium chloride in step 2 of the revised BCR sequential extraction protocol for soil and sediment?

C.M. Davidson, A.S. Hursthouse, D.M. Tognarelli, A.M. Ure, G.J. Urquhart

Research output: Contribution to journalArticle

38 Citations (Scopus)

Abstract

The revised, four-step BCR sequential extraction for soil or sediment has been compared with an alternative procedure in which 0.2 mol 1(-1) ammonium oxalate (pH 3) replaced 0.5 mol 1(-1) hydroxylammonium chloride (pH 1.5) in step 2, the reducible step. A variety of substrates were studied: BCR CRM601, a sewage sludge amended soil, two industrial soils, and a steel manufacturing by-product (basic oxygen furnace filter cake). Greater amounts of iron were recovered in step 2 when acid ammonium oxalate was used, for all substrates. Similar trends were observed for copper. Manganese and zinc were not strongly affected by the procedural modification, except for zinc in the two industrial soils, where oxalate extraction proved more efficient than use of hydroxylammonium chloride. A large proportion of the calcium and lead isolated in step 2 of the BCR procedure was not released until step 3 when the alternative procedure with oxalate in step 2 was used. This is probably due to rapid precipitation of analyte oxalates from solution. Thus, whilst oxalate offers superior dissolution of iron-containing matrix components, it should not be used if calcium or lead concentrations are to be measured. Selection of the most appropriated sequential extraction protocol for use in a particular study must always be carried out on the basis of 'fitness for purpose' criteria. However, the revised BCR protocol, involving use of 0.5 mol 1(-1) (NH2OHHCI)-H-. in the reducible step, appears to be more generally applicable than procedures involving acid ammonium oxalate. (C) 2003 Elsevier B.V. All rights reserved.
LanguageEnglish
Pages193-199
Number of pages6
JournalAnalytica Chimica Acta
Volume508
Issue number2
DOIs
Publication statusPublished - 22 Apr 2004

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Oxalic Acid
Hydroxylamine
Oxalates
oxalate
Sediments
Soil
ammonium
chloride
Soils
Acids
acid
Sewage
sediment
Zinc
Iron
soil
Calcium
Basic oxygen converters
Steel
Sewage sludge

Keywords

  • heavy metal analysis
  • soil
  • sequential extraction
  • BCR
  • acid ammonium oxalate
  • CERTIFICATION
  • IMPROVEMENT
  • SPECIATION
  • METALS

Cite this

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title = "Should acid ammonium oxalate replace hydroxylammonium chloride in step 2 of the revised BCR sequential extraction protocol for soil and sediment?",
abstract = "The revised, four-step BCR sequential extraction for soil or sediment has been compared with an alternative procedure in which 0.2 mol 1(-1) ammonium oxalate (pH 3) replaced 0.5 mol 1(-1) hydroxylammonium chloride (pH 1.5) in step 2, the reducible step. A variety of substrates were studied: BCR CRM601, a sewage sludge amended soil, two industrial soils, and a steel manufacturing by-product (basic oxygen furnace filter cake). Greater amounts of iron were recovered in step 2 when acid ammonium oxalate was used, for all substrates. Similar trends were observed for copper. Manganese and zinc were not strongly affected by the procedural modification, except for zinc in the two industrial soils, where oxalate extraction proved more efficient than use of hydroxylammonium chloride. A large proportion of the calcium and lead isolated in step 2 of the BCR procedure was not released until step 3 when the alternative procedure with oxalate in step 2 was used. This is probably due to rapid precipitation of analyte oxalates from solution. Thus, whilst oxalate offers superior dissolution of iron-containing matrix components, it should not be used if calcium or lead concentrations are to be measured. Selection of the most appropriated sequential extraction protocol for use in a particular study must always be carried out on the basis of 'fitness for purpose' criteria. However, the revised BCR protocol, involving use of 0.5 mol 1(-1) (NH2OHHCI)-H-. in the reducible step, appears to be more generally applicable than procedures involving acid ammonium oxalate. (C) 2003 Elsevier B.V. All rights reserved.",
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Should acid ammonium oxalate replace hydroxylammonium chloride in step 2 of the revised BCR sequential extraction protocol for soil and sediment? / Davidson, C.M.; Hursthouse, A.S.; Tognarelli, D.M.; Ure, A.M.; Urquhart, G.J.

In: Analytica Chimica Acta, Vol. 508, No. 2, 22.04.2004, p. 193-199.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Should acid ammonium oxalate replace hydroxylammonium chloride in step 2 of the revised BCR sequential extraction protocol for soil and sediment?

AU - Davidson, C.M.

AU - Hursthouse, A.S.

AU - Tognarelli, D.M.

AU - Ure, A.M.

AU - Urquhart, G.J.

PY - 2004/4/22

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N2 - The revised, four-step BCR sequential extraction for soil or sediment has been compared with an alternative procedure in which 0.2 mol 1(-1) ammonium oxalate (pH 3) replaced 0.5 mol 1(-1) hydroxylammonium chloride (pH 1.5) in step 2, the reducible step. A variety of substrates were studied: BCR CRM601, a sewage sludge amended soil, two industrial soils, and a steel manufacturing by-product (basic oxygen furnace filter cake). Greater amounts of iron were recovered in step 2 when acid ammonium oxalate was used, for all substrates. Similar trends were observed for copper. Manganese and zinc were not strongly affected by the procedural modification, except for zinc in the two industrial soils, where oxalate extraction proved more efficient than use of hydroxylammonium chloride. A large proportion of the calcium and lead isolated in step 2 of the BCR procedure was not released until step 3 when the alternative procedure with oxalate in step 2 was used. This is probably due to rapid precipitation of analyte oxalates from solution. Thus, whilst oxalate offers superior dissolution of iron-containing matrix components, it should not be used if calcium or lead concentrations are to be measured. Selection of the most appropriated sequential extraction protocol for use in a particular study must always be carried out on the basis of 'fitness for purpose' criteria. However, the revised BCR protocol, involving use of 0.5 mol 1(-1) (NH2OHHCI)-H-. in the reducible step, appears to be more generally applicable than procedures involving acid ammonium oxalate. (C) 2003 Elsevier B.V. All rights reserved.

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KW - soil

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KW - acid ammonium oxalate

KW - CERTIFICATION

KW - IMPROVEMENT

KW - SPECIATION

KW - METALS

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