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Phosphorus-31 Nuclear Magnetic Resonance Spectral Assignments of Phosphorus Compounds in Soil NaOH–EDTA Extracts

Benjamin L. Turner*,a, Nathalie Mahieub and Leo M. Condronc

a USDA–ARS, Northwest Irrigation and Soils Research Laboratory, 3793 N. 3600 E., Kimberly, ID 83341
b Dep. of Chemistry, Queen Mary, University of London, London E1 4NS, UK
c Soil, Plant, and Ecological Sciences Division, P.O. Box 84, Lincoln University, Canterbury, New Zealand



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Fig. 1. Solution 31P NMR spectra of model inorganic P compounds added to a soil extract (0.25 M NaOH and 0.05 M EDTA) that had been lyophilized and redissolved in D2O and 1 M NaOH.

 


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Fig. 2. Solution 31P NMR spectra of model orthophosphate monoesters added to a soil extract (0.25 M NaOH and 0.05 M EDTA) that had been lyophilized and redissolved in D2O and 1 M NaOH.

 


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Fig. 3. Solution 31P NMR spectra of model orthophosphate diesters added to a soil extract (0.25 M NaOH and 0.05 M EDTA) that had been lyophilized and redissolved in D2O and 1 M NaOH.

 


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Fig. 4. Solution 31P NMR spectra of model phosphonates added to a soil extract (0.25 M NaOH and 0.05 M EDTA) that had been lyophilized and redissolved in D2O and 1 M NaOH.

 


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Fig. 5. Solution 31P NMR spectra of model organic polyphosphates added to a soil extract (0.25 M NaOH and 0.05 M EDTA) that had been lyophilized and redissolved in D2O and 1 M NaOH.

 


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Fig. 6. Solution 31P NMR spectra of aromatic orthophosphate esters used in the measurement of phosphatase activity added to a soil extract (0.25 M NaOH and 0.05 M EDTA) that had been lyophilized and redissolved in D2O and 1 M NaOH. The methylumbelliferyl compounds were dissolved in D2O and 1 M NaOH only.

 


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Fig. 7. Degradation of organic P compounds in bacteria cultured from an upland blanket peat between 0 and 23 d after preparation. Bacteria were added to an alkaline soil extract (0.25 M NaOH and 0.05 M EDTA) that had been lyophilized and redissolved in D2O and 1 M NaOH.

 


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Fig. 8. The effect of probe temperature on (a) spectral areas of model P compounds in a synthetic mixture of 1 M NaOH (proportion of the initial spectral area at 19°C) and (b) proportion of the spectra assigned to the various functional P classes in a 0.25 M NaOH and 0.05 M EDTA soil extract (%). The regression lines on Fig. 3b describe the following models: [Proportion of orthophosphate (%)] = 53.49 ± 1.36 - 0.188 ± 0.051[probe temperature (°C)], R2 = 0.69, F = 13.6, P = 0.010; [Proportion of orthophosphate monoesters (%)] = 41.08 ± 1.83 + 0.165 ± 0.069[probe temperature (°C)], R2 = 0.49, F = 5.78, P = 0.053.

 





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