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High resolution characterization of organic phosphorus in soil extracts using 2D 1H-31P NMR correlation spectroscopy
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Ecology and Environmental Sciences.
Umeå University, Faculty of Science and Technology, Department of Ecology and Environmental Sciences.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
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2012 (English)In: Environmental Science and Technology, ISSN 0013-936X, E-ISSN 1520-5851, Vol. 46, no 7, 3950-3956 p.Article in journal (Refereed) Published
Abstract [en]

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, <sup>31</sup>P 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 multi-dimensional NMR methods to resolve overlapping <sup>31</sup>P signals. Using the new protocol on samples from two boreal humus soils with different Fe contents, two-dimensional <sup>1</sup>H-<sup>31</sup>P correlation spectra allowed unambiguous identification of a large number of P species based on their <sup>31</sup>P and <sup>1</sup>H 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.

Place, publisher, year, edition, pages
American Chemical Society (ACS), 2012. Vol. 46, no 7, 3950-3956 p.
National Category
Environmental Engineering Environmental Sciences related to Agriculture and Land-use
Identifiers
URN: urn:nbn:se:umu:diva-53091DOI: 10.1021/es204016hISI: 000302850400048PubMedID: 22394413OAI: oai:DiVA.org:umu-53091DiVA: diva2:509644
Available from: 2012-03-13 Created: 2012-03-13 Last updated: 2017-12-07Bibliographically approved
In thesis
1. Analysis and speciation of organic phosphorus in environmental matrices: Development of methods to improve 31P NMR analysis
Open this publication in new window or tab >>Analysis and speciation of organic phosphorus in environmental matrices: Development of methods to improve 31P NMR analysis
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Phosphorus (P) is an essential element for life on our planet. It is central in numerous biochemical processes in terrestrial and aqueous ecosystems including food production; and it is the primary growth-limiting nutrient in some of the world’s biomes. The main source of P for use as agricultural fertilizer is mining of non-renewable mineral phosphate. In terrestrial ecosystems the main source is soil P, where the largest fraction is organic P, composed of many species with widely differing properties. This fraction controls the utilization of P by plants and microorganisms and influences ecosystem development and productivity. However, there is only scarce knowledge about the molecular composition of the organic P pool, about the processes controlling its bioavailability, and about its changes as soils develop. Therefore, the aim of this thesis was to develop robust solution- and solid-state 31P nuclear magnetic resonance spectroscopy (NMR) methods to provide molecular information about speciation of the organic P pool, and to study its dynamics in boreal and tropical soils. By studying humus soils of a groundwater recharge/discharge productivity gradient in a Fennoscandian boreal forest by solution- and solid-state NMR, it was found that P speciation changed with productivity. In particular, the level of orthophosphate diesters decreased with increasing productivity while mono-esters such as inositol phosphates increased. Because the use of solution NMR on conventional NaOH/EDTA extracts of soils was limited due to severe line broadening caused by the presence of paramagnetic metal ions, a new extraction method was developed and validated. Based on the removal of these paramagnetic impurities by sulfide precipitation, a dramatic decrease in NMR linewidths was obtained, allowing for the first time to apply modern multi-dimensional solution NMR techniques to soil extracts. Identification of individual soil P-species, and tracking changes in the organic P pools during soil development provided information for connecting P-speciation to bioavailability and ecosystem properties. Using this NMR approach we studied the transformation of organic P in humus soils along a chronosequence (7800 years) in Northern Sweden. While total P varied little, the composition of the soil P pool changed particularly among young sites, where also the largest shift in the composition of the plant community and of soil microorganisms was observed. Very old soils, such as found Africa, are thought to strongly adsorb P, limiting plant productivity. I used NMR to study the effect of scattered agroforestry trees on P speciation in two semi-arid tropical woodlands with different soil mineralogy (Burkina Faso). While the total P concentration was low, under the tree canopies higher amounts of P and higher diversity of P-species were found, presumably reflecting higher microbial activity.

Place, publisher, year, edition, pages
Umeå: Umeå Universitet, 2014. 58 p.
Keyword
Phosphorus, soil, 31P NMR, NaOH/EDTA, terrestrial, sulfide, speciation, bioavailability, paramagnetic, humus, boreal, tropical, multi-dimensional, agroforestry, chronosequence
National Category
Physical Chemistry
Research subject
Physical Chemistry
Identifiers
urn:nbn:se:umu:diva-93409 (URN)978-91-7601-132-4 (ISBN)
Public defence
2014-10-17, KBC-huset, Stora hörsalen, KB3B1, KBC huset, s-90187, Umeå, 10:00 (English)
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Note

I delarbete III har titel och författaruppgifter förändrats.

Available from: 2014-09-26 Created: 2014-09-19 Last updated: 2014-09-24Bibliographically approved

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Vestergren, JohanVincent, Andrea GJansson, MatsPersson, PerGröbner, GerhardGiesler, ReinerSchleucher, Jürgen

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Vestergren, JohanVincent, Andrea GJansson, MatsPersson, PerGröbner, GerhardGiesler, ReinerSchleucher, Jürgen
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Department of ChemistryDepartment of Ecology and Environmental SciencesDepartment of Medical Biochemistry and Biophysics
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