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th  - 1988 - 51st ENC Conference

th  - 1988 - 51st ENC Conference

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144 I<br />

I IH AND 13C REFOCUSED GRADIENT IMAGING OF SOLIDS<br />

J. B. Miller* and A. N. Garroway<br />

Naval Research Laboratory, Code 6120<br />

Washington, DC 20375-5000<br />

We have previously demonstrated a technique for removing<br />

distortions from NMR images due to chemical shift and susceptibility<br />

effects which we call refocused gradient imaging (RGI). The technique<br />

relies on <strong>th</strong>e Carr-Purcell pulse sequence to refocus <strong>th</strong>e chemical-<br />

shift-like evolution of <strong>th</strong>e spins. The sign of <strong>th</strong>e gradient is<br />

switched synchronously wi<strong>th</strong> <strong>th</strong>e rf pulses so <strong>th</strong>at gradient evolution<br />

is not refocused.<br />

Here we extend refocused gradient imaging to <strong>th</strong>e observation of<br />

solids. For high natural abundance spins where <strong>th</strong>e homonuclear<br />

dipole-dipole interaction dominates, <strong>th</strong>e Carr-Purcell sequence is<br />

replaced by a pulse sequence which simultaneously refocuses <strong>th</strong>e<br />

dipolar and chemical-shift-like interactions. For low natural<br />

abundance spins <strong>th</strong>e Carr-Purcell sequence is used. Where necessary,<br />

high power decoupling of heteronuclei may be added.<br />

We describe <strong>th</strong>e pulse sequences used for RGI of solids and show<br />

examples of bo<strong>th</strong> IH and 13C images. The relative merits of IH and<br />

13C RGI are discussed. We find <strong>th</strong>at because of differences in<br />

experimental parameters and more efficient line-narrowing for 13C RGI,<br />

<strong>th</strong>e low natural abundance of 13C is not a severe limitation for carbon<br />

imaging of solids.<br />

145 I<br />

DERIVATION OF POLYMER RI~IEOLOGICAL CONSTANTS<br />

FROM THE VISCOSITY AND TEMPERATURE DEPEND<strong>ENC</strong>E OF xsC NMP.<br />

RELAXATION PARAMETERS: Anita J. Brandolini, Mobil Chemical<br />

Company, Edison Laboratory, P.O. Box 240, Edison, New<br />

Jersey 08818<br />

NMR relaxation parameters characterize polymer chain<br />

motions on a local scale; <strong>th</strong>eological constants describe<br />

<strong>th</strong>e viscoelastic properties of a bulk material.<br />

CorrelatinE bulk property measurements wi<strong>th</strong> spectroscopic<br />

data enables one to determine <strong>th</strong>e contribution of local<br />

seEmental reorientations to overall chain motions. The<br />

IsC NMR llnewid<strong>th</strong>s of low molecular-weight<br />

polyisobutylenes exhibit power-law dependences on sample<br />

viscosity. The exponent, which is different for each<br />

carbon type (quaternary, me<strong>th</strong>ylene, and me<strong>th</strong>yl), specifies<br />

<strong>th</strong>e fractional contribution of each carbon type to <strong>th</strong>e<br />

polymer's free volume and monomeric friction coefficient.<br />

Fur<strong>th</strong>ermore, <strong>th</strong>e IsC NMR linewid<strong>th</strong>s have a<br />

Williams-Landel-Ferry (WLF) dependence on temperature,<br />

which is <strong>th</strong>e same form observed for <strong>th</strong>e temperature<br />

variation of many bulk viscoelastic properties. The<br />

derived values for free volume and <strong>th</strong>ermal expansion<br />

coefficient aEree wi<strong>th</strong> published rheological parameters to<br />

wi<strong>th</strong>in ±10%.<br />

171

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