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An improved technique for the determination of organic phosphorus in sediments and soils by 31P nuclear magnetic resonance spectroscopy
Authors:R W McDowell  I Stewart
Institution:  a AgResearch Ltd, Invermay Agricultural Centre, Mosgiel, New Zealand b Department of Chemistry, University of Otago, Dunedin, New Zealand
Abstract:Knowledge of organic phosphorus (P) species quantity and distribution in sediments and soils is needed to determine the potential for aquatic and terrestrial organism growth. This can be achieved with 31P nuclear magnetic resonance spectroscopy (NMR), but resolving peaks within spectra can be problematic because of broadening via paramagnetics, which can cause peaks to overlap. We compared 31P NMR spectra of NaOH-EDTA extracts of three sediments and three soils to those that had first been pre-treated with Ca-EDTA-dithionite to remove Fe and Mn, paramagnetics that cause broadening of peaks, but leave organic P alone. Broadening of peaks in Ca-EDTA-dithionite pre-treated samples decreased by 46% and revealed peaks that were hidden compared to untreated samples. The spectrum of one pre-treated soil was similar if not better than the same soil that had received pre-treatment with Chelex resin (also to remove paramagnetics). Therefore, pre-treatment with Ca-EDTA-dithionite is recommended as a simple and cost-effective method for improving organic P idenTIFication and determination in subsequent NaOH-EDTA extracts of sediments and soils rich in Fe and Mn.
Keywords:31P NMR  Monoesters  Diesters  Paramagnetics  Broadening
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