Abstraet.A method for NMR investigations of surface nuclei using cross polarization from optically polarized xenon (OPCP) is descfibed. We find this methodology results in enhancement faetors of approximately 103 upon application to surface protons. The dynamics of 129Xe transfer to protons is examined in some detail, including the time, temperature, and multiple contact dependences of signal intensities. Furthermore, we diseuss the sensitivity of the transfer process to spatial diffusion. Finally, we report on application of the OPCP experiment to a low total surface area sample.
I. IntroduetionSolid-state NMR is a useful technique for investigating the structure and dynamics of bulk materials; however, because of its low sensitivity, its utility for studying surfaces has been limited to high surface area materials such as zeolites [1][2][3].In addition to the problem of sensitivity, selectivity, i.e. the problem of distinguishing surface from bulk species, is also an issue. Cross polarization (CP) [4] has been used successfully to selectively probe surface nuclei when the magnetization source, usually protons, resides exclusively at the surface. Maciel and Sindorf have utilized 1H-29Si CP-MAS to investigate the resonances of surface silicon atoms in silica [5]. Oldfield and coworkers used 1H-170 CP to observe surface hydroxyl groups of high surface area metal oxides that are difficult to detect by conventional NMR [6]. This technique is also useful for investigating interfaces. Zumbulyadis and O'Reilly have used lH-29Si CP to estimate the proximity of the backbone of a polymer to the surface of silica [7].