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Title: Synthesis and characterization of low-OH-fluor-chlorapatite: A single-crystal XRD and NMR spectroscopic study

Abstract

Los-OH apatite of the compositional range Ca{sub 4.99-5.06}(PO{sub 4}){sub 2.98-3.00}F{sub 0.51-0.48}Cl{sub 0.38-0.36}OH{sub 0.14-0.12} was synthesized and characterized structurally by synchrotron-based single-crystal X-ray diffraction (XRD), and multiple nuclear magnetic resonance (NMR) spectroscopic techniques. the average structure is hexagonal with space group P6{sub 3}/m. The presence of scattering in the single-crystal diffraction data set, which is incommensurate within the average hexagonal structure, suggests the presence of localized short-range monoclinic domains. Complex lineshapes in the {sup 31}P and {sup 19}F MAS NMR spectra are also consistent with the presence of an incommensurate phase. No evidence was detected for splitting of the Ca2 site into two distinct sites (as had been previously reported for hexagonal ternary apatities). Structure refinement and {sup 19}F{l_brace}{sup 35}Cl{r_brace} TRAPDOR NMR experiments verified intercolumnal neighboring of F and Cl atoms (inter-column distance of 2.62 {angstrom}) within this low-OH{sup -} apatite suggesting that long-range neighboring of F and Cl within the apatite anion channels is feasible.

Authors:
; ; ; ; ; ;  [1]
  1. SBU
Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Sponsoring Org.:
USDOE
OSTI Identifier:
1006739
Resource Type:
Journal Article
Journal Name:
American Mineralogist
Additional Journal Information:
Journal Volume: 93; Journal Issue: (1) ; 01, 2008; Journal ID: ISSN 0003-004X
Country of Publication:
United States
Language:
ENGLISH
Subject:
58 GEOSCIENCES; ANIONS; APATITES; ATOMS; DIFFRACTION; MONOCRYSTALS; NMR IMAGING; NMR SPECTRA; NUCLEAR MAGNETIC RESONANCE; SCATTERING; SPACE GROUPS; SPECTROSCOPY; SYNTHESIS; X-RAY DIFFRACTION

Citation Formats

McCubbin, Francis M, Mason, Harris E, Park, Hyunsoo, Phillips, Brian L, Parise, John B, Nekvasil, Hanna, and Lindsley, Donald H. Synthesis and characterization of low-OH-fluor-chlorapatite: A single-crystal XRD and NMR spectroscopic study. United States: N. p., 2008. Web. doi:10.2138/am.2008.2557.
McCubbin, Francis M, Mason, Harris E, Park, Hyunsoo, Phillips, Brian L, Parise, John B, Nekvasil, Hanna, & Lindsley, Donald H. Synthesis and characterization of low-OH-fluor-chlorapatite: A single-crystal XRD and NMR spectroscopic study. United States. https://doi.org/10.2138/am.2008.2557
McCubbin, Francis M, Mason, Harris E, Park, Hyunsoo, Phillips, Brian L, Parise, John B, Nekvasil, Hanna, and Lindsley, Donald H. 2008. "Synthesis and characterization of low-OH-fluor-chlorapatite: A single-crystal XRD and NMR spectroscopic study". United States. https://doi.org/10.2138/am.2008.2557.
@article{osti_1006739,
title = {Synthesis and characterization of low-OH-fluor-chlorapatite: A single-crystal XRD and NMR spectroscopic study},
author = {McCubbin, Francis M and Mason, Harris E and Park, Hyunsoo and Phillips, Brian L and Parise, John B and Nekvasil, Hanna and Lindsley, Donald H},
abstractNote = {Los-OH apatite of the compositional range Ca{sub 4.99-5.06}(PO{sub 4}){sub 2.98-3.00}F{sub 0.51-0.48}Cl{sub 0.38-0.36}OH{sub 0.14-0.12} was synthesized and characterized structurally by synchrotron-based single-crystal X-ray diffraction (XRD), and multiple nuclear magnetic resonance (NMR) spectroscopic techniques. the average structure is hexagonal with space group P6{sub 3}/m. The presence of scattering in the single-crystal diffraction data set, which is incommensurate within the average hexagonal structure, suggests the presence of localized short-range monoclinic domains. Complex lineshapes in the {sup 31}P and {sup 19}F MAS NMR spectra are also consistent with the presence of an incommensurate phase. No evidence was detected for splitting of the Ca2 site into two distinct sites (as had been previously reported for hexagonal ternary apatities). Structure refinement and {sup 19}F{l_brace}{sup 35}Cl{r_brace} TRAPDOR NMR experiments verified intercolumnal neighboring of F and Cl atoms (inter-column distance of 2.62 {angstrom}) within this low-OH{sup -} apatite suggesting that long-range neighboring of F and Cl within the apatite anion channels is feasible.},
doi = {10.2138/am.2008.2557},
url = {https://www.osti.gov/biblio/1006739}, journal = {American Mineralogist},
issn = {0003-004X},
number = (1) ; 01, 2008,
volume = 93,
place = {United States},
year = {Fri Dec 12 00:00:00 EST 2008},
month = {Fri Dec 12 00:00:00 EST 2008}
}