Research Article

Environmentally friendly flame retardants. A detailed solid-state NMR study of melamine orthophosphate

  1. Andreas Brinkmann1,*,
  2. Victor M. Litvinov2,
  3. Arno P. M. Kentgens1

Article first published online: 21 DEC 2007

DOI: 10.1002/mrc.2159

Issue

Magnetic Resonance in Chemistry

Magnetic Resonance in Chemistry

Special Issue: New techniques in solid-state NMR

Volume 45, Issue S1, pages S231–S246, December 2007

Additional Information

How to Cite

Brinkmann, A., Litvinov, V. M. and Kentgens, A. P. M. (2007), Environmentally friendly flame retardants. A detailed solid-state NMR study of melamine orthophosphate. Magn. Reson. Chem., 45: S231–S246. doi: 10.1002/mrc.2159

Author Information

  1. 1

    Physical Chemistry/Solid State NMR, Institute for Molecules and Materials, Radboud University Nijmegen, Toernooiveld 1, 6525 ED Nijmegen, The Netherlands

  2. 2

    Solid-State NMR, DSM Resolve, 6160 MD Geleen, The Netherlands

*Physical Chemistry/Solid State NMR, Institute for Molecules and Materials, Radboud University Nijmegen, Toernooiveld 1, 6525 ED Nijmegen, The Netherlands.

Publication History

  1. Issue published online: 21 DEC 2007
  2. Article first published online: 21 DEC 2007
  3. Manuscript Accepted: 2 NOV 2007
  4. Manuscript Revised: 30 OCT 2007
  5. Manuscript Received: 16 JUL 2007

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Keywords:

  • solid-state NMR;
  • 1H;
  • 13C;
  • 15N;
  • 31P;
  • environmentally friendly flame retardants;
  • melamine phosphates;
  • heteronuclear correlation spectroscopy;
  • homonuclear double-quantum spectroscopy;
  • distance measurements

Abstract

We used solid-state NMR spectroscopy to gain detailed information about the proton positions, proximities and the hydrogen-bonding network in the environmentally friendly flame retardant melamine orthophosphate (MP). High-resolution proton one- and two-dimensional solid-state NMR spectra were obtained at high external magnetic field in combination with fast magic angle spinning of the sample. Furthermore, we recorded homo- and heteronuclear correlation spectra of types 15N[BOND]15N, 1H[BOND]13C, 1H[BOND]15N and 1H[BOND]31P. In addition, we determined the geometry of the NH and NH2 groups in MP by 15N[BOND]1H heteronuclear recoupling experiments. We were able to completely assign the different isotropic chemical shifts in MP. Furthermore, we could identify the protonation of the melamine and orthophosphate moieties. The experimental results are discussed in connection with the structural model obtained by powder X-ray diffraction together with a combined molecular modeling-Rietveld refinement approach (De Ridder et al. Helv. Chim. Acta 2004; 87: 1894). We show that the geometry of the NH2 groups can only be successfully estimated by solid-state NMR. Copyright © 2007 John Wiley & Sons, Ltd.

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