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Solid State ³¹Phosphorus Nuclear Magnetic Resonance of Iron-, Manganese-, and Copper-Containing Synthetic Hydroxyapatites

^a National Research Council, NASA, Ames Research Center, Moffett Field, CA 94035
^b Dep. of Soil and Crop Sciences, Texas A&M Univ., College Station, TX 77843
^c NASA Johnson Space Center, Houston, TX 77058

View larger version (23K): [in a new window]   Fig. 1. X-ray diffraction patterns of pure-synthetic hydroxyaptite (SHA) and Mn11-SHA with the primary SHA diffraction peaks (hkl) labeled.

View larger version (38K): [in a new window]   Fig. 2. 31Phosphorus NMR spectra (2.0 kHz spin frequency) of: (a) pure-, Cu12-, Cu20-, Fe12-, Fe25-, Mn11-, and Mn24-synthetic hydroxyapatite (SHA); and (b) pure-SHA and pure-SHA mixed with 1.0 wt.% of MnSO4·H2O (Mn-mix), ferrihydrite (5Fe2O3·9H2O) (Fe-mix), Cu(NO3)2·2.5H2O (Cu-mix), and MgSO4 (Mg-mix). Spectral intensities were scaled for ease of comparison.

View larger version (33K): [in a new window]   Fig. 3. Inversion recovery stacked 31P spectra of: (a) pure-SHA and; (b) Mn11-SHA. Arrows indicate spectra closest to zero magnetization.

View larger version (30K): [in a new window]   Fig. 4. 31Phosphorus NMR signals passing through zero magnetization of pure-, Cu12-, Cu20-, Fe12-, Fe25-, Mn11- and Mn24-SHA after being treated 4 h with DTPA.

View larger version (59K): [in a new window]   Fig. 5. 31Phosphorus magnetization recovery curves as a function of time for: (a) pure synthetic hydroxyapatite (SHA) and the mixture of MnSO4·H2O and pure-SHA (Mn-mix); (b) all the Metal-synthetic hydroxyapatites; and (c) Fe12-, Mn11-, and Cu12-SHA after being treated 4 h with DTPA.

View larger version (10K): [in a new window]   Fig. 6. The linearized form of the spin-lattice relaxation equation as a function of time for: (a) pure-SHA and (b) Fe12-SHA. The solid line indicated where spin-diffusion was controlling 31P relaxation in pure-SHA and Fe12-SHA. Points that deviated from the solid line at early times in Fe12-SHA indicated where paramagnetic effects from Fe3+ were controlling 31P relaxation.