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th  - 1987 - 51st ENC Conference

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WF54 - POSTERS<br />

2D EXCHANGE NMR IN NON-SPINNING POWDERS<br />

C. Schmidt~ S. Kaufmann~ S. Wefing~ D. Theimer,<br />

B. Bl~mich" and H. W. Spiess~<br />

Max-Planck-Institut f~r Polymerforschung~<br />

Postfach 3148, D-6500 Mainz<br />

Information about molecular motions in isotropic<br />

solids is typically derived from lineshape analyses of<br />

wideline NMR spectra~ Nhile in liquid samples 2D exchange<br />

NMR has become an accepted me<strong>th</strong>od. In 2D exchange spectra<br />

some of <strong>th</strong>e information hidden in <strong>th</strong>e lineshapes of 1D<br />

spectra is reencoded into frequency coordinates of<br />

exchange signals, where it is accessible more accurately<br />

and in a model-independent fashion.<br />

We have studied deuteron and C-13 2D exchange NMR<br />

for <strong>th</strong>e characterization of molecular motions in powders<br />

and amorphous solid samples. The deuteron quadrupole<br />

coupling tensor is axially symmetric, so <strong>th</strong>at particu-<br />

larly simple exchange signals result. Discrete jumps are<br />

characterized by elliptical exchange singularities, where<br />

<strong>th</strong>e excentricity of <strong>th</strong>e ellipse is a direct measure of<br />

<strong>th</strong>e jump angle. Diffusive motions result in homogeneous<br />

broadening wi<strong>th</strong>.characteristic 2D lineshapes discrimina-<br />

ting different stages of partial diffusion towards <strong>th</strong>e<br />

full diffusion limit. For short mixing times pure<br />

diffusion~ diffusion in connection wi<strong>th</strong> discrete jumps,<br />

and pure jump motions can be distinguished.<br />

The 2D exchange experiment can also be performed in<br />

C-13 NMR on selectively labelled compounds. The asymmetry<br />

of <strong>th</strong>e chemical shielding tensor, however~ leads to more<br />

complicated 2D exchange patterns. Experimental and <strong>th</strong>eo-<br />

retical data demonstrate <strong>th</strong>at <strong>th</strong>e wideline 2D exchange<br />

experiment produces a direct image of <strong>th</strong>e jump angle<br />

distribution.<br />

Ref erences:<br />

1) C. Schmidt, S. Wefing~ B. Bl~mich and H.'W. Spiess,<br />

Chem. Phys. Lett. 130, 84 (198b).<br />

2) M. Linder, A. Hbhener and R. R. Ernst~ J. Chem. Phys.<br />

73, 4959 ~1980).

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