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DIVISION S-2—SOIL CHEMISTRY

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

* Corresponding author (bsutter{at}mail.arc.nasa.gov)

The incorporation of micronutrients into synthetic hydroxyapatite (SHA) is proposed for slow release of these nutrients to crops in the National Aeronautics and Space Administration's (NASA's) Advanced Life Support (ALS) program for Lunar or Martian outposts. Solid state ³¹P nuclear magnetic resonance (NMR) was utilized to examine the paramagnetic effects of Fe³⁺, Mn²⁺, and Cu²⁺ to determine if they were incorporated into the SHA structure. Separate Fe³⁺, Mn²⁺, and Cu²⁺ containing SHA materials along with a transition metal free SHA (pure-SHA) were synthesized using a precipitation method. The proximity (<1 nm) of the transition metals to the ³¹P nuclei of SHA were apparent when comparing the integrated ³¹P signal intensities of the pure-SHA (87 arbitrary units g^-1) with the Fe-, Mn-, and Cu-SHA materials (37–71 arbitrary units g^-1). The lower integrated ³¹P signal intensities of the Fe-, Mn-, and Cu-SHA materials relative to the pure-SHA suggested that Fe³⁺, Mn²⁺, and Cu²⁺ were incorporated in the SHA structure. Further support for Fe³⁺, Mn²⁺, and Cu²⁺ incorporation was demonstrated by the reduced spin-lattice relaxation constants of the Fe-, Mn-, and Cu-SHA materials relative to pure-SHA . Inversion recovery spectra indicated that Fe³⁺, Mn²⁺, and Cu²⁺ were not homogeneously distributed about the ³¹P nuclei in the SHA structure. Extraction with diethylene-triamine-penta-acetic acid (DTPA) suggested that between 50 and 80% of the total starting metal concentrations were incorporated in the SHA structure. Iron-, Mn-, and Cu-containing SHA are potential slow release sources of Fe, Mn, and Cu in the ALS cropping system.

Abbreviations: ALS, Advanced Life Support • DTPA, diethylene-triamine-penta-acetic acid • IR, infrared • NASA, National Aeronautics and Space Administration • NMR, nuclear magnetic resonance • SHA, synthetic hydroxyapatite • XRD, x-ray diffraction

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