New methods for the acquisition of ultra-wideline solid-state NMR spectra of spin-1/2 nuclides.
The Wideband Uniform Rate Smooth Truncation - Carr-Purcell Meiboom-Gill (WURST-CPMG) pulse sequence was recently introduced as a new method of acquiring ultra-wideline solid-state NMR (SSNMR) patterns of quadrupolar nuclei (Chem. Phys. Lett. 464 (2008) 97). Herein, we describe the application of the WURST-CPMG pulse sequence to stationary samples (i.e., non-spinning or "static" samples) of various spin-1/2 nuclides ((119)Sn, (207)Pb, (199)Hg and (195)Pt) in order to examine its effectiveness for acquiring ultra-wideline SSNMR patterns. WURST-CPMG is compared to the CPMG and Cross Polarization (CP)-CPMG pulse sequences in select cases ((119)Sn and (207)Pb, respectively), and its usefulness in obtaining ultra-wideline SSNMR spectra in a piecewise fashion is explored. In addition, a preliminary investigation of pulses generated using optimal control theory (OCT) for the purpose of wideline excitation is presented; spectra acquired using these pulses are compared with standard, rectangular pulses of similar pulse powers. Both methods show much promise for acquiring high quality wideline patterns dominated by chemical shift anisotropy, with minimal distortions and significantly reduced experimental times.
Department of Chemistry and Biochemistry, University of Windsor, Windsor, Ontario, Canada N9B 3P4.
Alan W
AW
MacGregor
Luke A
LA
O'Dell
Robert W
RW
Schurko
D000465:Algorithms; D003198:Computer Simulation; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008956:Models, Chemical; D011868:Radioisotopes / Q000032:analysis* / Q000737:chemistry*; D013113:Spin Labels
D011868:Radioisotopes; D013113:Spin Labels