Sensitivity enhancement of double quantum NMR spectroscopy by modified CPMG

A modified Carr-Purcell-Meiboom-Gill (CPMG) sequence for sensitivity enhancement of dipolar coupled homonuclear spin pairs in static solid-state NMR is presented. The modified CPMG block uses the Hahn-solid-Hahn echo as basic element of the CPMG echo train to refocus the homonuclear dipolar coupling and chemical shift anisotropy. The new CPMG sequence is dubbed as Hahn-solid-Hahn Carr-Purcell-Meiboom-Gill (HSHCPMG). We demonstrate a gain in signal to noise ratio of approximately 4.2 using HSHCPMG sequence in double quantum filtered CP experiment for 5%-(13)C(2)-(15)N-glycine. The resulting gain in sensitivity in the spikelet spectrum does not compromise the anisotropic information that is available from static NMR lineshapes. As an example, relative orientation angles of chemical shift anisotropy tensors for the alpha and carbonyl carbons in glycine are determined from the 2D DOQSY experiment recorded with the HSHCPMG block in the acquisition dimension. The resultant relative orientation angles of the two CSA tensors are compared to those obtained from 2D DOQSY experiment acquired without sensitivity enhancement as well as to the data as available from single crystal NMR experiments.