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High-Resolution Characterization of Organic Phosphorus in Soil Extracts Using 2D H-1-P-31 NMR Correlation Spectroscopy

Vestergren, Johan; Vincent, Andrea G.; Jansson, Mats; Persson, Per LU ; Istedt, Ulrik; Groebner, Gerhard; Giesler, Reiner and Schleucher, Juergen (2012) In Environmental Science & Technology 46. p.3950-3956
Abstract
Organic phosphorus (P) compounds represent a major component of soil P in many soils and are key sources of P for microbes and plants. Solution NMR (nuclear magnetic resonance spectroscopy) is a powerful technique for characterizing organic P species. However, P-31 NMR spectra are often complicated by overlapping peaks, which hampers identification and quantification of the numerous P species present in soils. Overlap is often exacerbated by the presence of paramagnetic metal ions, even if they are in complexes with EDTA following NaOH/EDTA extraction. By removing paramagnetic impurities using a new precipitation protocol, we achieved a dramatic improvement in spectral resolution. Furthermore, the obtained reduction in line widths enabled... (More)
Organic phosphorus (P) compounds represent a major component of soil P in many soils and are key sources of P for microbes and plants. Solution NMR (nuclear magnetic resonance spectroscopy) is a powerful technique for characterizing organic P species. However, P-31 NMR spectra are often complicated by overlapping peaks, which hampers identification and quantification of the numerous P species present in soils. Overlap is often exacerbated by the presence of paramagnetic metal ions, even if they are in complexes with EDTA following NaOH/EDTA extraction. By removing paramagnetic impurities using a new precipitation protocol, we achieved a dramatic improvement in spectral resolution. Furthermore, the obtained reduction in line widths enabled the use of multidimensional NMR methods to resolve overlapping P-31 signals. Using the new protocol on samples from two boreal humus soils with different Fe contents, 2D H-1-P-31 correlation spectra allowed unambiguous identification of a large number of P species based on their P-31 and H-1 chemical shifts and their characteristic coupling patterns, which would not have been possible using previous protocols. This approach can be used to identify organic P species in samples from both terrestrial and aquatic environments increasing our understanding of organic P biogeochemistry. (Less)
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author
publishing date
type
Contribution to journal
publication status
published
subject
in
Environmental Science & Technology
volume
46
pages
3950 - 3956
publisher
The American Chemical Society
external identifiers
  • scopus:84859298288
ISSN
1520-5851
DOI
10.1021/es204016h
language
English
LU publication?
no
id
e8286a97-bc95-4d73-b344-4c7680efad12 (old id 4332237)
date added to LUP
2014-03-04 09:45:17
date last changed
2017-08-27 04:53:46
@article{e8286a97-bc95-4d73-b344-4c7680efad12,
  abstract     = {Organic phosphorus (P) compounds represent a major component of soil P in many soils and are key sources of P for microbes and plants. Solution NMR (nuclear magnetic resonance spectroscopy) is a powerful technique for characterizing organic P species. However, P-31 NMR spectra are often complicated by overlapping peaks, which hampers identification and quantification of the numerous P species present in soils. Overlap is often exacerbated by the presence of paramagnetic metal ions, even if they are in complexes with EDTA following NaOH/EDTA extraction. By removing paramagnetic impurities using a new precipitation protocol, we achieved a dramatic improvement in spectral resolution. Furthermore, the obtained reduction in line widths enabled the use of multidimensional NMR methods to resolve overlapping P-31 signals. Using the new protocol on samples from two boreal humus soils with different Fe contents, 2D H-1-P-31 correlation spectra allowed unambiguous identification of a large number of P species based on their P-31 and H-1 chemical shifts and their characteristic coupling patterns, which would not have been possible using previous protocols. This approach can be used to identify organic P species in samples from both terrestrial and aquatic environments increasing our understanding of organic P biogeochemistry.},
  author       = {Vestergren, Johan and Vincent, Andrea G. and Jansson, Mats and Persson, Per and Istedt, Ulrik and Groebner, Gerhard and Giesler, Reiner and Schleucher, Juergen},
  issn         = {1520-5851},
  language     = {eng},
  pages        = {3950--3956},
  publisher    = {The American Chemical Society},
  series       = {Environmental Science & Technology},
  title        = {High-Resolution Characterization of Organic Phosphorus in Soil Extracts Using 2D H-1-P-31 NMR Correlation Spectroscopy},
  url          = {http://dx.doi.org/10.1021/es204016h},
  volume       = {46},
  year         = {2012},
}