Unexpected structural/motional mode of water intercalated into an α-crystalline zirconium phosphate deduced by 31P and 2H solid-state MAS NMR spectra

Bakhmutov, Vladimir I.; Contreras‐Ramirez, Aida; Banerjee, Sayan; Zhou, Hong‐Cai

doi:10.1002/mrc.5225

Unexpected structural/motional mode of water intercalated into an α-crystalline zirconium phosphate deduced by ³¹P and ²H solid-state MAS NMR spectra

Journal Article · Wed Oct 06 00:00:00 EDT 2021 · Magnetic Resonance in Chemistry

DOI:https://doi.org/10.1002/mrc.5225· OSTI ID:1976359

^[1]; Contreras‐Ramirez, Aida ^[2]; Banerjee, Sayan ^[2]; Zhou, Hong‐Cai ^[2]

Texas A & M University, College Station, TX (United States); OSTI
Texas A & M University, College Station, TX (United States)

Here, in developing the approach to understanding dynamics of intercalates in layered materials, crystalline-layered zirconium phosphate Zr (HPO₄)₂·0.35D2O has been prepared and characterized by the ¹H, ³¹P, and ²H solid-state MAS NMR spectra, including ³¹P and ²H T₁ measurements. At temperatures >253 K, the intercalated water shows two spectrally-distinguished deuterons unprecedentedly with different DQCC's and ²H T₁ times, one of which is hydrogen bonded. The collected data allowed to identify an unexpected bonding/dynamic mode of water molecules, which experience fast rotation around the hydrogen bond, formed with a zirconium-coordinated oxygen. The low-temperature ²H MAS NMR experiments have demonstrated the presence of additional hydrogen bond P—(H)O˙˙˙ DO, population of which grows on cooling to 195 K corresponding to the doubly hydrogen-bonded immobile water molecule.

View Accepted Manuscript (DOE)

Research Organization:: Texas A & M University, College Station, TX (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES); Robert A. Welch Foundation

Grant/Contract Number:: SC0017864

OSTI ID:: 1976359

Alternate ID(s):: OSTI ID: 1826628

Journal Information:: Magnetic Resonance in Chemistry, Journal Name: Magnetic Resonance in Chemistry Journal Issue: 2 Vol. 60; ISSN 0749-1581

Publisher:: WileyCopyright Statement

Country of Publication:: United States

Language:: English

References (24)

Adsorption of aqueous Pb(II), Cu(II), Zn(II) ions by amorphous tin(VI) hydrogen phosphate: an excellent inorganic adsorbent Zhu, C.; Dong, X.; Chen, Z. International Journal of Environmental Science and Technology, Vol. 13, Issue 5 https://doi.org/10.1007/s13762-016-0964-9	journal	March 2016
Deuteron magnetic resonance studies of water associated with phospholipids Salsbury, N. J.; Darke, A.; Chapman, D. Chemistry and Physics of Lipids, Vol. 8, Issue 2 https://doi.org/10.1016/0009-3084(72)90026-6	journal	March 1972
Synthetic inorganic ion-exchange materials—I zirconium phosphate Amphlett, C. B.; McDonald, L. A.; Redman, M. J. Journal of Inorganic and Nuclear Chemistry, Vol. 6, Issue 3 https://doi.org/10.1016/0022-1902(58)80152-9	journal	June 1958
The preparation of crystalline zirconium phosphate and some observations on its ion exchange behaviour Clearfield, A.; Stynes, J. A. Journal of Inorganic and Nuclear Chemistry, Vol. 26, Issue 1 https://doi.org/10.1016/0022-1902(64)80238-4	journal	January 1964
A 1H NMR relaxation time study of dynamic processes in zirconium phosphates of differing crystallinities and in related compounds Slade, R.; Forano, C.; Peraio, A. Solid State Ionics, Vol. 61, Issue 1-3 https://doi.org/10.1016/0167-2738(93)90330-6	journal	May 1993
An approach to increase the permselectivity and mono-valent ion selectivity of cation-exchange membranes by introduction of amorphous zirconium phosphate nanoparticles Golubenko, D. V.; Karavanova, Yu. A.; Melnikov, S. S. Journal of Membrane Science, Vol. 563 https://doi.org/10.1016/j.memsci.2018.06.024	journal	October 2018
Selective ion-exchange separation of scandium(III) over iron(III) by crystalline α-zirconium phosphate platelets under acidic conditions Avdibegović, Dženita; Zhang, Wenzhong; Xu, Junhua Separation and Purification Technology, Vol. 215 https://doi.org/10.1016/j.seppur.2018.12.079	journal	May 2019
Zirconium Phosphate: The Pathway from Turbostratic Disorder to Crystallinity Contreras-Ramirez, Aida; Tao, Songsheng; Day, Gregory S. Inorganic Chemistry, Vol. 58, Issue 20 https://doi.org/10.1021/acs.inorgchem.9b02442	journal	October 2019
Thermodynamic and Spectroscopic Analyses of Zirconium Phosphate-Absorbed Ammonia Yamaguchi, Masakuni; Miyaoka, Hiroki; Kojima, Yoshitsugu The Journal of Physical Chemistry C, Vol. 125, Issue 7 https://doi.org/10.1021/acs.jpcc.0c10882	journal	February 2021
³¹ P NMR Relaxation and Motions of Phosphate Groups in Layered Zirconium Phosphate Materials Bakhmutov, Vladimir I.; Clearfield, Abraham The Journal of Physical Chemistry C, Vol. 120, Issue 34 https://doi.org/10.1021/acs.jpcc.6b06417	journal	August 2016
Role of ion exchange in solid-state chemistry Clearfield, Abraham Chemical Reviews, Vol. 88, Issue 1 https://doi.org/10.1021/cr00083a007	journal	January 1988
Phosphorus-31 solid-state NMR studies of the structure of amine-intercalated .alpha.-zirconium phosphate. 2. Titration of .alpha.-zirconium phosphate with n-propylamine and n-butylamine MacLachlan, Dugald J.; Morgan, Keith R. The Journal of Physical Chemistry, Vol. 96, Issue 8 https://doi.org/10.1021/j100187a053	journal	April 1992
Observation of molecular reorientation in ice by proton and deuterium magnetic resonance Wittebort, R. J.; Usha, M. G.; Ruben, D. J. Journal of the American Chemical Society, Vol. 110, Issue 17 https://doi.org/10.1021/ja00225a013	journal	August 1988
ADSORPTION ON INORGANIC MATERIALS. I. CATION EXCHANGE PROPERTIES OF ZIRCONIUM PHOSPHATE ¹ Kraus, Kurt A.; Phillips, Harold O. Journal of the American Chemical Society, Vol. 78, Issue 3 https://doi.org/10.1021/ja01584a053	journal	February 1956
Proton Chemical Shift Tensors and Hydrogen Bond Geometry: A ¹ H− ² H Dipolar NMR Study of the Water Molecule in Crystalline Hydrates Wu, Gang; Freure, Christopher J.; Verdurand, Elodie Journal of the American Chemical Society, Vol. 120, Issue 50 https://doi.org/10.1021/ja983126t	journal	December 1998
Water Confinement in Faujasite Cages: A Deuteron NMR Investigation in a Wide Temperature Range. 1. Low Temperature Spectra Szymocha, A. M.; Birczyński, A.; Lalowicz, Z. T. The Journal of Physical Chemistry A, Vol. 118, Issue 29 https://doi.org/10.1021/jp504648s	journal	July 2014
Freezing Point Depression of Water in Phospholipid Membranes: A Solid-State NMR Study Lee, Dong-Kuk; Kwon, Byung Soo; Ramamoorthy, Ayyalusamy Langmuir, Vol. 24, Issue 23 https://doi.org/10.1021/la8023698	journal	November 2008
An NMR study on the mechanisms of freezing and melting of water confined in spherically mesoporous silicas SBA-16 Miyatou, Tatsuya; Ohashi, Ryutaro; Ida, Tomonori Physical Chemistry Chemical Physics, Vol. 18, Issue 27 https://doi.org/10.1039/C6CP03111K	journal	January 2016
Recent advances in solid-state NMR spectroscopy of quadrupolar nuclei Ashbrook, Sharon E. Physical Chemistry Chemical Physics, Vol. 11, Issue 32 https://doi.org/10.1039/b907183k	journal	January 2009
High-resolution 2H solid-state NMR of 2H2O adsorbed onto activated carbon Harris, Robin K.; Thompson, Timothy V.; Norman, Paul R. Journal of the Chemical Society, Faraday Transactions, Vol. 91, Issue 12 https://doi.org/10.1039/ft9959101795	journal	January 1995
Deuteron Magnetic Resonance in Polycrystalline Heavy Ice (D ₂ O) Jackson, Jasper A.; Rabideau, Sherman W. The Journal of Chemical Physics, Vol. 41, Issue 12 https://doi.org/10.1063/1.1725860	journal	December 1964
Deuteron Magnetic Resonance Study of Barium Chlorate Monohydrate Chiba, Takehiko The Journal of Chemical Physics, Vol. 39, Issue 4 https://doi.org/10.1063/1.1734396	journal	August 1963
Direct observation of tetrahedral hydrogen jumps in ice Ih Fujara, F.; Wefing, S.; Kuhs, W. F. The Journal of Chemical Physics, Vol. 88, Issue 11 https://doi.org/10.1063/1.454426	journal	June 1988
A proton T ₁ -nuclear magnetic resonance dispersion study of water motion in snowflakes and hexagonal ice Westlund, Per-Olof Molecular Physics, Vol. 117, Issue 7-8 https://doi.org/10.1080/00268976.2018.1541197	journal	October 2018

Similar Records

Elucidating structure and dynamics of crystalline α-zirconium phosphates intercalated with water and methanol by multinuclear solid-state MAS NMR: A comprehensive NMR approach

Journal Article · Sun Feb 27 23:00:00 EST 2022 · Magnetic Resonance in Chemistry · OSTI ID:1976360

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
NMR
dynamics
relaxation
structural elucidation
zirconium phosphates

Unexpected structural/motional mode of water intercalated into an α-crystalline zirconium phosphate deduced by 31P and 2H solid-state MAS NMR spectra

Citation Formats

References (24)

Similar Records

Related Subjects

Unexpected structural/motional mode of water intercalated into an α-crystalline zirconium phosphate deduced by ³¹P and ²H solid-state MAS NMR spectra