Solid‐state lead‐207 NMR of lead(II) nitrate: Localized heating effects at high magic angle spinning speeds

Gorkom, Leon C.M. Van; Hook, James M.; Logan, Michael; Hanna, John V.; Wasylishen, Roderick E.

doi:10.1002/mrc.1260331005

Cited by 126 publications

(160 citation statements)

References 35 publications

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“…Friction results in sample heating and temperature gradients across the sample, which leads to line broadening. [21][22][23][24] Nuclei such as 207 Pb have isotropic shifts with a pronounced temperature dependence. [24] The 207 Pb MAS spectra of Pb(NO 3 ) 2 ( Figure 6) show that different spinning 207 Pb MAS spectra of Pb(NO 3 ) 2 recorded at different spinning rates, which lead to different temperature gradients across the sample.…”

Section: Sasa Antonijevic and Geoffrey Bodenhausen*mentioning

confidence: 99%

High‐Resolution NMR Spectroscopy in Solids by Truly Magic‐Angle Spinning

Antonijevic

Bodenhausen

2005

Angew Chem Int Ed

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Right angles: In solid‐state magic‐angle spinning (MAS) NMR spectra, the line widths of carbonyl carbon atoms in polycrystalline cholesteryl acetate are found to be as narrow as 0.039 ppm if the magic angle is adjusted very accurately, that is, within ±0.004° (see picture). The line broadening observed for slightly miss‐set angles is mostly due to residual chemical shift anisotropy (CSA) interactions. Long spin‐echo life times up to ${{{\rm T}{{\prime \hfill \atop 2\hfill}}}}$=3.6 s open the way to sophisticated NMR methods.

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Section: Sasa Antonijevic and Geoffrey Bodenhausen*mentioning

confidence: 99%

High‐Resolution NMR Spectroscopy in Solids by Truly Magic‐Angle Spinning

Antonijevic

Bodenhausen

2005

Angew Chem Int Ed

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“…In addition to the concern for calibration of the thermocouple over the temperature range investigated, one must also consider frictional heating of the rotor resulting from aeorodynamic drag, radiofrequency induction heating resulting primarily from the 1 H decoupling, and Joule-Thompson cooling and heating (15). The solid-state 207 Pb chemical shift of lead nitrate serves as a convenient chemical shift thermometer, both for static and MAS measurements (16)(17)(18)(19)(20)(21)(22). A review of solid-state 207 Pb NMR spectroscopy, including a section on the lead shift as a thermometer, is given by Dybowski and Neue (23).…”

Section: Spectrometer Calibrationmentioning

confidence: 99%

¹³C CP/MAS: Application to glycine

Taylor

2004

Concepts Magnetic Resonance

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ABSTRACT:In a previous article (Concepts Magn Reson May, 2004), the initial setup of the 13 C CP/MAS experiment was described. The advantages of the experiment over direct 13 C excitation were also given. In this article, the experiment is applied to three polymorphic structures of glycine. Temperature calibration of the experiment to investigate molecular dynamics as a function of temperature is also described. While the 13 C CP/MAS experiment is widely applicable, it can not be universally used. The 13 C CP/MAS experiment works at ambient temperature for both the α and γ polymorphic structures of glycine. However, the cross-polarization technique fails to provide a signal at low temperature from either polymorph. The failure of the technique for both polymorphs arises from the shortened 1 H T 1ρ at low temperatures. This shortened T 1ρ results from the hindered rotation of the -NH 3 group. The technique even fails at ambient temperature for β glycine. Again, the reason is a shortened 1 H T 1ρ .

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“…Since all our NMR probes here will be isolated spin-1/2 nuclei, the exchange processes will affect the solid-state NMR spectra as follows. The methyl 13 C resonances of the XMe 3 groups will be affected by all three kinds of dynamic disorder. Internal reorientation of the XMe 3 groups will affect only the respective interchanging methyl 13 C resonances, not the NMR resonances of E and X.…”

Section: ±4mentioning

confidence: 99%

“…The methyl 13 C resonances of the XMe 3 groups will be affected by all three kinds of dynamic disorder. Internal reorientation of the XMe 3 groups will affect only the respective interchanging methyl 13 C resonances, not the NMR resonances of E and X. The resonances of E and X are both affected by n-fold orientational disorder and the X resonances by whole-molecule reorientational jumps, and thus they can serve as NMR probes for studying and distinguishing these processes.…”

Section: ±4mentioning

confidence: 99%