Local environment and composition of magnesium gallium layered double hydroxides determined from solid-state 1H and 71Ga NMR spectroscopy

Line Boisen Staal, Andrew S. Lipton, Vadim Zorin, Ulla Gro Nielsen

Research output: Contribution to journalJournal articleResearchpeer-review

Abstract

Ordering of gallium(III) in a series of magnesium gallium (MgGa) layered double hydroxides (LDHs), [Mg1−xGax(OH)2(NO3)x·yH2O] was investigated using solid-state 1H and 71Ga NMR spectroscopy as well as powder X-ray diffraction. Three different proton environments from Mg3single bondOH, Mg2Gasingle bondOH and intergallery water molecules were assigned and quantified using {1H,71Ga} HETCOR and 1H MAS NMR. A single 71Ga site originating from the unique Ga site in the MgGa LDH׳s was observed in 71Ga MAS and 3QMAS NMR spectra. Both 1H MAS NMR spectra recorded at 21.1 T (900 MHz) and elemental analysis show that the synthesized MgGa LDH׳s had a lower Mg:Ga ratio than that of the starting reactant solution. The origin of this is the formation of soluble [Ga(OH)4]− complexes formed during synthesis, and not due to formation of insoluble gallium (oxy)hydroxides. No sign of Gasingle bondOsingle bondGa connectivities or defects were detected for the MgGa LDH׳s.
Original languageEnglish
JournalJournal of Solid State Chemistry
Volume219
Pages (from-to)242-246
ISSN0022-4596
DOIs
Publication statusPublished - Nov 2014

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Hydroxides
Gallium
Magnesium
Nuclear magnetic resonance spectroscopy
hydroxides
gallium
magnesium
solid state
nuclear magnetic resonance
Chemical analysis
spectroscopy
Nuclear magnetic resonance
X ray powder diffraction
Protons
Defects
Molecules
protons
Water
defects
synthesis

Cite this

@article{6a39a9bf17004ca884252296bb0e836d,
title = "Local environment and composition of magnesium gallium layered double hydroxides determined from solid-state 1H and 71Ga NMR spectroscopy",
abstract = "Ordering of gallium(III) in a series of magnesium gallium (MgGa) layered double hydroxides (LDHs), [Mg1−xGax(OH)2(NO3)x·yH2O] was investigated using solid-state 1H and 71Ga NMR spectroscopy as well as powder X-ray diffraction. Three different proton environments from Mg3single bondOH, Mg2Gasingle bondOH and intergallery water molecules were assigned and quantified using {1H,71Ga} HETCOR and 1H MAS NMR. A single 71Ga site originating from the unique Ga site in the MgGa LDH׳s was observed in 71Ga MAS and 3QMAS NMR spectra. Both 1H MAS NMR spectra recorded at 21.1 T (900 MHz) and elemental analysis show that the synthesized MgGa LDH׳s had a lower Mg:Ga ratio than that of the starting reactant solution. The origin of this is the formation of soluble [Ga(OH)4]− complexes formed during synthesis, and not due to formation of insoluble gallium (oxy)hydroxides. No sign of Gasingle bondOsingle bondGa connectivities or defects were detected for the MgGa LDH׳s.",
author = "{Boisen Staal}, Line and Lipton, {Andrew S.} and Vadim Zorin and Nielsen, {Ulla Gro}",
year = "2014",
month = "11",
doi = "10.1016/j.jssc.2014.07.023",
language = "English",
volume = "219",
pages = "242--246",
journal = "Journal of Solid State Chemistry",
issn = "0022-4596",
publisher = "Heinemann",

}

Local environment and composition of magnesium gallium layered double hydroxides determined from solid-state 1H and 71Ga NMR spectroscopy. / Boisen Staal, Line; Lipton, Andrew S.; Zorin, Vadim; Nielsen, Ulla Gro.

In: Journal of Solid State Chemistry, Vol. 219, 11.2014, p. 242-246.

Research output: Contribution to journalJournal articleResearchpeer-review

TY - JOUR

T1 - Local environment and composition of magnesium gallium layered double hydroxides determined from solid-state 1H and 71Ga NMR spectroscopy

AU - Boisen Staal, Line

AU - Lipton, Andrew S.

AU - Zorin, Vadim

AU - Nielsen, Ulla Gro

PY - 2014/11

Y1 - 2014/11

N2 - Ordering of gallium(III) in a series of magnesium gallium (MgGa) layered double hydroxides (LDHs), [Mg1−xGax(OH)2(NO3)x·yH2O] was investigated using solid-state 1H and 71Ga NMR spectroscopy as well as powder X-ray diffraction. Three different proton environments from Mg3single bondOH, Mg2Gasingle bondOH and intergallery water molecules were assigned and quantified using {1H,71Ga} HETCOR and 1H MAS NMR. A single 71Ga site originating from the unique Ga site in the MgGa LDH׳s was observed in 71Ga MAS and 3QMAS NMR spectra. Both 1H MAS NMR spectra recorded at 21.1 T (900 MHz) and elemental analysis show that the synthesized MgGa LDH׳s had a lower Mg:Ga ratio than that of the starting reactant solution. The origin of this is the formation of soluble [Ga(OH)4]− complexes formed during synthesis, and not due to formation of insoluble gallium (oxy)hydroxides. No sign of Gasingle bondOsingle bondGa connectivities or defects were detected for the MgGa LDH׳s.

AB - Ordering of gallium(III) in a series of magnesium gallium (MgGa) layered double hydroxides (LDHs), [Mg1−xGax(OH)2(NO3)x·yH2O] was investigated using solid-state 1H and 71Ga NMR spectroscopy as well as powder X-ray diffraction. Three different proton environments from Mg3single bondOH, Mg2Gasingle bondOH and intergallery water molecules were assigned and quantified using {1H,71Ga} HETCOR and 1H MAS NMR. A single 71Ga site originating from the unique Ga site in the MgGa LDH׳s was observed in 71Ga MAS and 3QMAS NMR spectra. Both 1H MAS NMR spectra recorded at 21.1 T (900 MHz) and elemental analysis show that the synthesized MgGa LDH׳s had a lower Mg:Ga ratio than that of the starting reactant solution. The origin of this is the formation of soluble [Ga(OH)4]− complexes formed during synthesis, and not due to formation of insoluble gallium (oxy)hydroxides. No sign of Gasingle bondOsingle bondGa connectivities or defects were detected for the MgGa LDH׳s.

U2 - 10.1016/j.jssc.2014.07.023

DO - 10.1016/j.jssc.2014.07.023

M3 - Journal article

VL - 219

SP - 242

EP - 246

JO - Journal of Solid State Chemistry

JF - Journal of Solid State Chemistry

SN - 0022-4596

ER -