Efficient cross-polarization using a composite 0 degrees pulse for NMR studies on static solids.
In most solid-state NMR experiments, cross-polarization is an essential step to detect low-gamma nuclei such as (13)C and (15)N. In this study, we present a new cross-polarization scheme using spin-locks composed of composite 0 degrees pulses in the RF channels of high-gamma and low-gamma nuclei to establish the Hartmann-Hahn match. The composite 0 degrees pulses with no net nutation-angle{(2pi)(X)-(2pi)(-X)-(2pi)(Y)-(2pi)(-Y) -}(n) applied simultaneously to both high-gamma (I) and low-gamma (S) nuclei create an effective heteronuclear dipolar Hamiltonian H(d)((0))=d/2(2I(Z)S(Z)+I(X)S(X)+I(Y)S(Y)), which is capable of transferring the Z-component of the I spin magnetization to the Z-component of the S spin magnetization. It also retains a homonuclear dipolar coupling Hamiltonian that enables the flip-flop transfer among abundant spins. While our experimental results indicate that the new pulse sequence, called composite zero cross-polarization (COMPOZER-CP) performs well on adamantane, it is expected to be more valuable to study semi-solids like liquid crystalline materials and model lipid membranes. Theoretical analysis of COMPOZER-CP is presented along with experimental results. Our experimental results demonstrate that COMPOZER-CP overcomes the RF field inhomogeneity and Hartmann-Hahn mismatch for static solids. Experimental results comparing the performance of COMPOZER-CP with that of the traditional constant-amplitude CP and rampCP sequences are also presented in this paper.
Fukuchi
Masashi
M
Division of Chemistry, Graduate School of Science, Kyoto University, Kyoto 606-8502, Japan.
Ramamoorthy
Ayyalusamy
A
Takegoshi
K
K
D000218:Adamantane / Q000737:chemistry; D002247:Carbon Isotopes; D005454:Fluorescence Polarization; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008280:Magnetics; D008859:Microscopy, Polarization; D009584:Nitrogen; D011048:Polarography; D011846:Radio Waves
D002247:Carbon Isotopes; D009584:Nitrogen; D000218:Adamantane