Water Orientation in Smectites Using NMR Nutation Experiments

Fleury, Marc; Canet, Daniel

doi:10.1021/jp4118503

Cited by 11 publications

(11 citation statements)

References 19 publications

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“…By contrast, the same field cycling spectrometers become inefficient for quadrupolar nuclei (spin I > 1/2) because of the large enhancement of their relaxation rates under confinement. In that context, spin-locking relaxation measurement [77][78][79][80] is a powerful tool since it may be performed with usual spectrometer and is simply limited by the short dead time required to generate a sequence of NMR pulses (typically, micro-seconds).…”

Section: Nuclear Magnetic Resonance Relaxometrymentioning

confidence: 99%

“…Three specific angles (0 • , 30 • , and 90 • ) are then selected to determine the time evolution of four independent coherences (labeled T 11 (s), T 21 (a), T 21 (s), and T 22 (a) [82][83][84] under spin-locking conditions by applying an irradiation field of calibrated irradiation power ω 1 . For I = 1/2 spin nuclei, such spin-locking relaxometry measurements probe only a single angular velocity (2 ω 1 ) for each irradiation power [77][78][79]. By contrast, in the presence of a residual quadrupolar coupling (ω Q ), I = 1 spin nuclei probe three different angular velocities:…”

Section: Nuclear Magnetic Resonance Relaxometrymentioning

confidence: 99%

See 1 more Smart Citation

Water and Ion Dynamics in Confined Media: A Multi-Scale Study of the Clay/Water Interface

Porion

Asaad

Dabat

et al. 2021

Colloids and Interfaces

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This review details a large panel of experimental studies (Inelastic Neutron Scattering, Quasi-Elastic Neutron Scattering, Nuclear Magnetic Resonance relaxometry, Pulsed-Gradient Spin-Echo attenuation, Nuclear Magnetic Resonance Imaging, macroscopic diffusion experiments) used recently to probe, over a large distribution of characteristic times (from pico-second up to days), the dynamical properties of water molecules and neutralizing cations diffusing within clay/water interfacial media. The purpose of this review is not to describe these various experimental methods in detail but, rather, to investigate the specific dynamical information obtained by each of them concerning these clay/water interfacial media. In addition, this review also illustrates the various numerical methods (quantum Density Functional Theory, classical Molecular Dynamics, Brownian Dynamics, macroscopic differential equations) used to interpret these various experimental data by analyzing the corresponding multi-scale dynamical processes. The purpose of this multi-scale study is to perform a bottom-up analysis of the dynamical properties of confined ions and water molecules, by using complementary experimental and numerical studies covering a broad range of diffusion times (between pico-seconds up to days) and corresponding diffusion lengths (between Angstroms and centimeters). In the context of such a bottom-up approach, the numerical modeling of the dynamical properties of the diffusing probes is based on experimental or numerical investigations performed on a smaller scale, thus avoiding the use of empirical or fitted parameters.

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Section: Nuclear Magnetic Resonance Relaxometrymentioning

confidence: 99%

Section: Nuclear Magnetic Resonance Relaxometrymentioning

confidence: 99%

Water and Ion Dynamics in Confined Media: A Multi-Scale Study of the Clay/Water Interface

Porion

Asaad

Dabat

et al. 2021

Colloids and Interfaces

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“…However, such analysis can only be performed if all layers are oriented with respect to the magnetic field and in the case of 'clean' systems containing a small amount of or no paramagnetic impurities. Without the need for clay-layer orientation, a new technique (Fleury and Canet, 2014) allows the observation and quantification of oriented water within the interlayer as a function of relative humidity and type of ions. Despite the random orientation of the clay layers within the powder, the resulting signal is different from water interacting with the solid and one can deduce the relative amount of these two-proton populations.…”

Section: Water In the Interlayer Space Of Smectitesmentioning

confidence: 99%

Water mobility and structure in natural clay systems

Fleury¹,

Kohler²,

Barré³

2016

Filling the Gaps - From Microscopic Pore Structures to Transport Properties In Shales

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From current and previous work by the present authors, experimental results showing the connectivity and the water mobility in natural clay systems are emphasized. Using various low-field Nuclear Magnetic Resonance techniques, a large range of time-and length scales, from nm to cm, can be explored. The amount of water in the interlayer space of smectites at different relative humidities can be detected and quantified. Simple criteria such as unimodal or multimodal relaxation time distributions give a simple and quick indication of connectivity between different porosity compartments. A new technique has allowed the orientation of water in the interlayer space of smectites to be determined; from 39 to 66% of the water molecules are noted as being 'oriented.'

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“…This feature has been exploited in various studies dealing with water in clays. [7][8][9][10][11] A nutation experiment consists of observing the motion of nuclear magnetization in the presence of a radiofrequency (rf) field B 1 applied continuously. Viewed from the so-called rotating frame (the frame rotating around the direction of the static magnetic field B 0 , at the frequency of the rf field), this motion is similar to precession as it is merely a rotation around the B 1 field which is stationary in the rotating frame.…”

Section: Introductionmentioning

confidence: 99%

Longitudinal relaxation rate measurements for different signals unveiled by nutation spectroscopy: Application to the characterization of two arrangements experienced by water in a clay network

Ferrari

Moyne

Canet

2021

Magnetic Reson in Chemistry

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Nutation consists in monitoring the motion of nuclear magnetization under the application of a radiofrequency (rf) field. With an appropriate amplitude of the rf field, the nutation frequency depends on the NMR relaxation times. This property offers the possibility of differentiating species having the same Larmor frequency but differing by their relaxation times. This may occur for the composite proton NMR signal of water in complex systems. Separate nutation signals are thus observed with the possibility of measuring their longitudinal relaxation times by simply applying a saturation hard pulse, followed by an evolution interval, prior to the nutation sequence. This novel experiment has been used for studying the two sites existing for water in two kaolinite samples (one hydrated after stabilization of several months and the other nonhydrated). It turns out that water in these two sites differs essentially by its transverse relaxation time. Moreover, recovery is surprisingly biexponential for these two signals. A proper analysis of results obtained by this saturationrecovery nutation experiment provides not only the specific longitudinal relaxation rates of water in these two sites but also information about the averaging which occurs at long evolution times. This is discussed with regard of the structure and organization of the clay network. In particular, from relaxation rates at short evolution times, it is shown that this network is mainly constituted of ordered platelets, with a relatively weak proportion of randomly distributed platelets.

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Water Orientation in Smectites Using NMR Nutation Experiments

Cited by 11 publications

References 19 publications

Water and Ion Dynamics in Confined Media: A Multi-Scale Study of the Clay/Water Interface

Water and Ion Dynamics in Confined Media: A Multi-Scale Study of the Clay/Water Interface

Water mobility and structure in natural clay systems

Longitudinal relaxation rate measurements for different signals unveiled by nutation spectroscopy: Application to the characterization of two arrangements experienced by water in a clay network

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