Measurement of dilute 29Si species in solution using a large volume coil and DEFT NMR

A large-sample-volume nuclear magnetic resonance (NMR) spectroscopy probehead has been developed for the detection and characterization of low concentrations of 29Si species in aqueous solution. The approach described entails the use of a large-diameter radio frequency solenoid coil that permits substantially larger sample volumes to be investigated at moderate magnetic field strengths, compared with conventional NMR probehead configurations. In addition, difficulties presented by long 29Si T1 relaxation times have been circumvented by using the DEFT NMR pulse sequence, which permits more rapid signal averaging. Through a combination of these hardware and methodological improvements, high-resolution 29Si NMR spectra have been obtained at 4.2 T (29Si resonance frequency = 36.8 MHz) for an 800 microM solution of 96% 29Si-enriched silicic acid, H4SiO4 (pH approximately 8), with a signal-to-noise ratio of 16 and a line width of 31 Hz after 3 h of total measurement time.