Negassa,W. and Kruse,J.(2010): Phosphorus speciation in agro-industrial byproducts: Sequential fractionation, solution 31P NMR, and P K- and L2,3-edge XANES spectroscopy. Environ. Sci. Technol., 44, 2092-2097.

『農業−産業副産物におけるリン化学種同定:連続分別および溶液31PのNMR(核磁気共鳴)法およびPのK-端とL2,3-端XANES(X線吸収端近傍構造)分光法』


(Abstract)
 Little is known about P species in agro-industrial byproducts from developing countries, which may be either pollutants or valuable soil amendments. The present study speciated P in dry (COD) and wet (COW) coffee, sisal (SIS), barley malt (BEB) and sugar cane processing (FIC) byproducts, and filter cakes of linseed (LIC) and niger seed (NIC) with sequential fractionation, solution 31P nuclear magnetic resonance (NMR) spectroscopy, and P K- and L2,3-edge X-ray absorption near-edge structure (XANES) spectroscopy. The sequential P fractionation recovered 59% to almost 100% of total P (Pt), and more than 50% of Pt was extracted by H2O and NaHCO3 in five out of seven samples. Similarly, the NaOH + EDTA extraction for solution 31P NMR recovered 48-94% of Pt. The 31P NMR spectra revealed orthophosphate (6-81%), pyrophosphate (0-10%), and orthophosphate monoesters (6-94%). Orthophosphate predominated in COD, COW, SIS. and FIC, whereas BEB, LIC, and NIC were rich orthophosphate monoesters. The concentrations of Pi and Po determined in the sequential and NaOH + EDTA extractions and 31P NMR spectra were strongly and positively correlated (r = 0.88-1.99). Furthermore, the P K- and L2,3-edge XANES confirmed the H2SO4-Pi detected in the sequential fractionation by unequivocal identification of Ca-P phases in a few samples. The results indicate that the combined use of all four analytical methods is crucial for comprehensive P speciation in environmental samples and the application of these byproducts to soil.』

Introduction
Materials and methods
 Sample collection and preparation
 Sequential P fractionation
 Solution 31P NMR analysis
 P L-edge X-ray Absorption Near-Edge Structure spectroscopy
 L2,3-edge X-ray Absorption Near-Edge Structure spectroscopy
Results and Discussion
 Sequentially extracted P fractions
 NaOH + EDTA-extracts and solution 31P NMR spectra
 P K- and L2,3-edge X-ray Absorption Near-Edge Structure spectroscopy
Acknowledgments
Supporting information available
Literature cited


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