skip to main content
DOE PAGES title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Computational and Experimental 1H-NMR Study of Hydrated Mg-Based Minerals

Abstract

Magnesium oxide (MgO) can convert to different magnesium-containing compounds depending on exposure and environmental conditions. Many MgO-based phases contain hydrated species allowing 1H-nuclear magnetic resonance (NMR) spectroscopy to be used in the characterization and quantification of proton-containing phases; however, surprisingly limited examples have been reported. Here, 1H-magic angle spinning (MAS) NMR spectra of select Mg-based minerals are presented and assigned. These experimental results are combined with computational NMR density functional theory (DFT) periodic calculations to calibrate the predicted chemical shielding results. This correlation is then used to predict the NMR shielding for a series of different MgO hydroxide, magnesium chloride hydrate, magnesium perchlorate, and magnesium cement compounds to aid in the future assignment of 1H-NMR spectra for complex Mg phases.

Authors:
; ; ORCiD logo
Publication Date:
Sponsoring Org.:
USDOE
OSTI Identifier:
1601894
Grant/Contract Number:  
[NA0003525]
Resource Type:
Published Article
Journal Name:
Molecules
Additional Journal Information:
[Journal Name: Molecules Journal Volume: 25 Journal Issue: 4]; Journal ID: ISSN 1420-3049
Publisher:
MDPI AG
Country of Publication:
Switzerland
Language:
English

Citation Formats

Sorte, Eric G., Rimsza, Jessica M., and Alam, Todd M. Computational and Experimental 1H-NMR Study of Hydrated Mg-Based Minerals. Switzerland: N. p., 2020. Web. doi:10.3390/molecules25040933.
Sorte, Eric G., Rimsza, Jessica M., & Alam, Todd M. Computational and Experimental 1H-NMR Study of Hydrated Mg-Based Minerals. Switzerland. doi:10.3390/molecules25040933.
Sorte, Eric G., Rimsza, Jessica M., and Alam, Todd M. Wed . "Computational and Experimental 1H-NMR Study of Hydrated Mg-Based Minerals". Switzerland. doi:10.3390/molecules25040933.
@article{osti_1601894,
title = {Computational and Experimental 1H-NMR Study of Hydrated Mg-Based Minerals},
author = {Sorte, Eric G. and Rimsza, Jessica M. and Alam, Todd M.},
abstractNote = {Magnesium oxide (MgO) can convert to different magnesium-containing compounds depending on exposure and environmental conditions. Many MgO-based phases contain hydrated species allowing 1H-nuclear magnetic resonance (NMR) spectroscopy to be used in the characterization and quantification of proton-containing phases; however, surprisingly limited examples have been reported. Here, 1H-magic angle spinning (MAS) NMR spectra of select Mg-based minerals are presented and assigned. These experimental results are combined with computational NMR density functional theory (DFT) periodic calculations to calibrate the predicted chemical shielding results. This correlation is then used to predict the NMR shielding for a series of different MgO hydroxide, magnesium chloride hydrate, magnesium perchlorate, and magnesium cement compounds to aid in the future assignment of 1H-NMR spectra for complex Mg phases.},
doi = {10.3390/molecules25040933},
journal = {Molecules},
number = [4],
volume = [25],
place = {Switzerland},
year = {2020},
month = {2}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record
DOI: 10.3390/molecules25040933

Save / Share:

Works referenced in this record:

Ultrathin hexagonal MgO nanoflakes coated medical textiles and their enhanced antibacterial activity
journal, October 2016

  • Ponnuvelu, Dinesh Veeran; Selvaraj, Aravind; Suriyaraj, Shanmugam Prema
  • Materials Research Express, Vol. 3, Issue 10
  • DOI: 10.1088/2053-1591/3/10/105005

Size-Dependent Optical Properties of MgO Nanocubes
journal, August 2005

  • Stankic, Slavica; Müller, Markus; Diwald, Oliver
  • Angewandte Chemie International Edition, Vol. 44, Issue 31
  • DOI: 10.1002/anie.200500663

Nonlinear optical response of Mg/MgO structures prepared by laser ablation method
journal, May 2017

  • Abrinaei, Fahimeh
  • Journal of the European Optical Society-Rapid Publications, Vol. 13, Issue 1
  • DOI: 10.1186/s41476-017-0042-z

Generalized Gradient Approximation Made Simple
journal, October 1996

  • Perdew, John P.; Burke, Kieron; Ernzerhof, Matthias
  • Physical Review Letters, Vol. 77, Issue 18, p. 3865-3868
  • DOI: 10.1103/PhysRevLett.77.3865

Nanorod-Superconductor Composites: A Pathway to Materials with High Critical Current Densities
journal, September 1996


High-Pressure δ-Al(OH) 3 and δ-AlOOH Phases and Isostructural Hydroxides/Oxyhydroxides:  New Structural Insights from High-Resolution 1 H and 27 Al NMR
journal, November 2007

  • Xue, Xianyu; Kanzaki, Masami
  • The Journal of Physical Chemistry B, Vol. 111, Issue 46
  • DOI: 10.1021/jp073968r

Micro-analysis of the role of interfacial transition zone in “salt weathering” on concrete
journal, November 2010


Hunting for hydrogen: random structure searching and prediction of NMR parameters of hydrous wadsleyite
journal, January 2016

  • Moran, Robert F.; McKay, David; Pickard, Chris J.
  • Physical Chemistry Chemical Physics, Vol. 18, Issue 15
  • DOI: 10.1039/C6CP01529H

Modelling one- and two-dimensional solid-state NMR spectra: Modelling 1D and 2D solid-state NMR spectra
journal, December 2001

  • Massiot, Dominique; Fayon, Franck; Capron, Mickael
  • Magnetic Resonance in Chemistry, Vol. 40, Issue 1
  • DOI: 10.1002/mrc.984

A Picture of Disorder in Hydrous Wadsleyite—Under the Combined Microscope of Solid-State NMR Spectroscopy and Ab Initio Random Structure Searching
journal, January 2019

  • McKay, David; Moran, Robert F.; Dawson, Daniel M.
  • Journal of the American Chemical Society, Vol. 141, Issue 7
  • DOI: 10.1021/jacs.8b11519

High fire resistance in blocks containing coal combustion fly ashes and bottom ash
journal, August 2011


QUANTUM ESPRESSO: a modular and open-source software project for quantum simulations of materials
journal, September 2009

  • Giannozzi, Paolo; Baroni, Stefano; Bonini, Nicola
  • Journal of Physics: Condensed Matter, Vol. 21, Issue 39, Article No. 395502
  • DOI: 10.1088/0953-8984/21/39/395502

Norm-conserving and ultrasoft pseudopotentials for first-row and transition elements
journal, October 1994


Hydration and Hydroxylation of MgO in Solution: NMR Identification of Proton-Containing Intermediate Phases
journal, January 2019


Characterization of hydrous species in minerals by high-speed proton MAS-NMR
journal, March 1988

  • Yesinowski, James P.; Eckert, Hellmut.; Rossman, George R.
  • Journal of the American Chemical Society, Vol. 110, Issue 5
  • DOI: 10.1021/ja00213a007

High-Resolution 1H NMR Spectroscopy in the Solid State: Very Fast Sample Rotation and Multiple-Quantum Coherences
journal, August 2001

  • Schnell, Ingo; Spiess, Hans Wolfgang
  • Journal of Magnetic Resonance, Vol. 151, Issue 2
  • DOI: 10.1006/jmre.2001.2336

Structural, morphological and optical properties of MgO nanoparticles for antibacterial applications
journal, March 2016


Water in the Earth's mantle: a solid-state NMR study of hydrous wadsleyite
journal, January 2013

  • Griffin, John M.; Berry, Andrew J.; Frost, Daniel J.
  • Chemical Science, Vol. 4, Issue 4
  • DOI: 10.1039/c3sc21892a

Combining solid-state NMR spectroscopy with first-principles calculations – a guide to NMR crystallography
journal, January 2016

  • Ashbrook, Sharon E.; McKay, David
  • Chemical Communications, Vol. 52, Issue 45
  • DOI: 10.1039/C6CC02542K

Electrical Characterization of GaN Metal Oxide Semiconductor Diodes Using MgO as the Gate Oxide
journal, January 2002

  • Kim, J.; Gila, B.; Mehandru, R.
  • Journal of The Electrochemical Society, Vol. 149, Issue 8
  • DOI: 10.1149/1.1489689

Role of magnesium fertilisers in agriculture: plant–soil continuum
journal, January 2015

  • Senbayram, Mehmet; Gransee, Andreas; Wahle, Verena
  • Crop and Pasture Science, Vol. 66, Issue 12
  • DOI: 10.1071/CP15104

Magnesium oxide clusters as promising candidates for hydrogen storage
journal, January 2019

  • Mojica-Sánchez, Juan Pablo; Zarate-López, Tania Isabel; Flores-Álvarez, José Manuel
  • Physical Chemistry Chemical Physics, Vol. 21, Issue 41
  • DOI: 10.1039/C9CP05075B

Light-induced conversion of an insulating refractory oxide into a persistent electronic conductor
journal, October 2002

  • Hayashi, Katsuro; Matsuishi, Satoru; Kamiya, Toshio
  • Nature, Vol. 419, Issue 6906
  • DOI: 10.1038/nature01053

XRD and 1H MAS NMR spectroscopic study of mixed oxides obtained by calcination of layered-double hydroxides
journal, December 2000


Temperature and common-ion effect on magnesium oxide (MgO) hydration
journal, April 2010


Decontamination of Chemical Warfare Agents [English]
journal, May 2010

  • Singh, Beer; Prasad, Gangavarapu; Pandey, K.
  • Defence Science Journal, Vol. 60, Issue 4
  • DOI: 10.14429/dsj.60.487

Crystallography Open Database – an open-access collection of crystal structures
journal, May 2009

  • Gražulis, Saulius; Chateigner, Daniel; Downs, Robert T.
  • Journal of Applied Crystallography, Vol. 42, Issue 4
  • DOI: 10.1107/S0021889809016690

Rectangular MgO microsheets with strong catalytic activity
journal, October 2011


All-electron magnetic response with pseudopotentials: NMR chemical shifts
journal, May 2001


Study of MgO and Pt/MgO Systems by XRD, TPR, and 1 H MAS NMR
journal, February 1999

  • Aramendía, María Angeles; Benítez, José Antonio; Borau, Victoriano
  • Langmuir, Vol. 15, Issue 4
  • DOI: 10.1021/la9808972

Performance Assessment in Support of the 1996 Compliance Certification Application for the Waste Isolation Pilot Plant
journal, October 1999


29 Si and 1 H NMR spectroscopy of high-pressure hydrous magnesium silicates
journal, April 1997

  • Phillips, Brian L.; Burnley, Pamela C.; Worminghaus, Karen
  • Physics and Chemistry of Minerals, Vol. 24, Issue 3
  • DOI: 10.1007/s002690050031

Study of the Structure of OH Groups on MgO by 1D and 2D 1 H MAS NMR Combined with DFT Cluster Calculations
journal, December 2007

  • Chizallet, Céline; Costentin, Guylène; Lauron-Pernot, Hélène
  • The Journal of Physical Chemistry C, Vol. 111, Issue 49
  • DOI: 10.1021/jp077089g

First-principles calculations of NMR parameters for phosphate materials
journal, September 2010

  • Vasconcelos, Filipe; Cristol, Sylvain; Paul, Jean-François
  • Magnetic Resonance in Chemistry, Vol. 48, Issue S1
  • DOI: 10.1002/mrc.2667

Quantitative description of 1 H SQ and DQ coherences for the hydroxyl disorder within hydrous ringwoodite
journal, January 2018

  • Grüninger, Helen; Schmutzler, Adrian; Siegel, Renée
  • Physical Chemistry Chemical Physics, Vol. 20, Issue 22
  • DOI: 10.1039/C8CP00863A

Characterization of Various Magnesium Oxides by XRD and1H MAS NMR Spectroscopy
journal, April 1999


Dynamics on the microsecond timescale in hydrous silicates studied by solid-state 2H NMR spectroscopy
journal, January 2010

  • Griffin, John M.; Miller, Andrew J.; Berry, Andrew J.
  • Physical Chemistry Chemical Physics, Vol. 12, Issue 12
  • DOI: 10.1039/b924666e

Models of Aged Magnesium–Silicate–Hydrate Cements Based on the Lizardite and Talc Crystals: A Periodic DFT-GIPAW Investigation
journal, March 2017

  • Pedone, Alfonso; Palazzetti, Federico; Barone, Vincenzo
  • The Journal of Physical Chemistry C, Vol. 121, Issue 13
  • DOI: 10.1021/acs.jpcc.7b00708

1H MAS NMR study of the coordination of hydroxyl groups generated upon adsorption of H2O and CD3OH on clean MgO surfaces
journal, July 2006


Calcium Phosphates and Hydroxyapatite: Solid-State NMR Experiments and First-Principles Calculations
journal, December 2007


1 H shielding anisotropy in Mg(OH) 2 : The isolated OH group
journal, February 1988

  • Sears, R. E. J.; Kaliaperumal, R.; Manogaran, S.
  • The Journal of Chemical Physics, Vol. 88, Issue 4
  • DOI: 10.1063/1.454062

Identification of the OH groups responsible for kinetic basicity on MgO surfaces by 1H MAS NMR
journal, November 2009

  • Chizallet, Céline; Petitjean, Hugo; Costentin, Guylène
  • Journal of Catalysis, Vol. 268, Issue 1
  • DOI: 10.1016/j.jcat.2009.09.003

The PAW/GIPAW approach for computing NMR parameters: A new dimension added to NMR study of solids
journal, July 2011