『Summary
Common sequential phosphorus (P) extraction methods are not specific
to particular chemical chemical species and have several limitations.
This work presents the first chemical method for quantification
of individual mineral and sorbed P species. It was developed by
combining a conversion technique with a sequential extraction
procedure. Mangrove sediments with different characteristics were
incubated in pH-adjusted 0.01 M CaCl2 with
and without reference material additions of octacalcium phosphate
(Ca8H2(PO4)6・5H2O; OCP), hydroxyapatite
(Ca5(PO4)3OH),
strengite (FePO4・2H2O)
or variscite (AlPO4・2H2O).
The changes in soluble phosphate concentration were measured in
the supernatant solution, while pH-induced variations in P composition
were determined by subsequent sequential extraction of the sediments.
Dissolved phosphate concentration was controlled by adsorption
below pH 7.8. Above this pH, soluble phosphate concentration was
governed by OCP, which was qualitatively determined by plotting
the experimental values of pH + pH2PO4 and pH - 0.5 pCa on a solubility diagram including
the isotherms of known crystalline phosphate compounds. In contrast
to the often-predicted slow dissolution rate of crystalline phosphates
in soils or sediments, drastic changes in P composition by dissolution,
precipitation and adsorption processes are detected after 7 days.
These were mainly not observed indirectly by changes in dissolved
phosphate through adsorption effects, but were determined quantitatively
by subsequent sequential extraction, thus enabling the quantification
of individual species. Evaluation of the method was performed
by standard addition experiments. Besides P species quantification,
the method provides the means for other applications, such as
the determination of P mineral dissolution kinetics in solids
and sediments, the prediction of P composition in changing environmental
settings and the refinement of theoretical models of phosphate
solubility in soil and sedimentary environments.』
Introduction
Materials and methods
Sediment sampling and preparation
Reference materials for standard addition experiments
Development of the CONVEX method
Method evaluation by standard addition experiments
Analytical methods and procedures
Results
CONVEX method: soluble phosphate data
CONVEX method: fractionation data
Calculation of the data for P species quantification
Discussion
Acknowledgements
References