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Improvement of 13 C and 15 N CPMAS NMR spectra of bulk soils, particle size fractions and organic material by treatment with 10% hydrofluoric acid
Abstract
Summary: The small organic matter content of mineral soils makes it difficult to obtain 13 C and 15 N nuclear magnetic resonance (NMR) spectra with acceptable signal‐to‐noise ratios. Subjecting such samples to hydrofluoric acid removes mineral matter and leads to a relative increase in organic material. The effect of treatment with 10% hydrofluoric acid on bulk chemical composition and resolution of solid‐state 13 C NMR spectra was investigated with six soils, some associated particle size fractions, plant litter and compost. The treatment enhanced the signal‐to‐noise ratio of the solid‐state 13 C NMR spectra. The improvement in spectrum quality was greatest in the clay fraction of soil contaminated with coal ash. The removal of paramagnetic compounds associated with the ash may be the main reason for the improvement. Based on total C, total N, C/N ratio and intensity distribution of the solid‐state 13 C NMR spectra, no changes in organic matter composition could be detected, except for a possible loss of carbohydrates. After treatment with HF, solid‐state 15 N NMR spectra of particle size fractions were obtained and indicated that the observable nitrogen is present mostly as peptides and free amino groups. Extraction with hydrofluoric acid is recommended as a routine treatment prior to solid‐state 13 C and 15 N NMR on soil containing little C or N and soil samples containing paramagnetic compounds from natural or anthropogenic sources.
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Cited by
Stability of organic carbon in deep soil layers controlled by fresh carbon supply
Fontaine, S., Barot, S., Barré, P., Bdioui, N., Mary, B., & Rumpel, C. (2007) · Nature · doi:10.1038/nature06275 · Cited by 2,279
Deep soil organic matter—a key but poorly understood component of terrestrial C cycle
Rumpel, C., & Kögel-Knabner, I. (2011) · Plant and Soil · doi:10.1007/s11104-010-0391-5 · Cited by 1,848
Self-citationSOM fractionation methods: Relevance to functional pools and to stabilization mechanisms
von Lützow, M., Kögel-Knabner, I., Ekschmitt, K., Flessa, H., Guggenberger, G., Matzner, E., & Marschner, B. (2007) · Soil Biology and Biochemistry · doi:10.1016/j.soilbio.2007.03.007 · Cited by 1,590
Cycling and composition of organic matter in terrestrial and marine ecosystems
Baldock, J. A., Masiello, C. A., Gélinas, Y., & Hedges, J. I. (2004) · Marine Chemistry · doi:10.1016/j.marchem.2004.06.016 · Cited by 414
Mueller, C. W., & Koegel-Knabner, I. (2009) · Biology and Fertility of Soils · doi:10.1007/s00374-008-0336-9 · Cited by 127
Metadata
- Authors
- SCHMIDT, M. W. I., KNICKER, H., HATCHER, P. G., & KOGEL‐KNABNER, I.
- Venue
- European Journal of Soil Science
- Publisher
- Wiley
- Published
- 1997-06
- Volume
- 48
- Issue
- 2
- Pages
- 319-328
- ISSN
- 1351-0754 (ISSN-L)
- 1365-2389
- OpenAlex
- W2168170151
- Cited by
- 401
- References
- 0
- FWCI
- 21.94
- Type
- journal article
- Language
- en
- Open access
- closed
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- SCHMIDT, M. W. I., KNICKER, H., HATCHER, P. G., & KOGEL‐KNABNER, I. (1997). Improvement of 13 C and 15 N CPMAS NMR spectra of bulk soils, particle size fractions and organic material by treatment with 10% hydrofluoric acid. European Journal of Soil Science. https://doi.org/10.1111/j.1365-2389.1997.tb00552.x
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