Achieving 1 ppm field homogeneity above 24 T: Application of differential mapping for shimming Keck and the Series Connected Hybrid magnets at the NHMFL.

Powered resistive and resistive-superconductive hybrid magnets can reach fields higher than superconducting NMR magnets but lack the field homogeneity and temporal stability needed for high resolution NMR. Due to field fluctuations in powered magnets, commercially available mapping systems fail to produce maps of these magnets with sufficient reproducibility, thus hampering attempts to improve homogeneity of the field they generate. Starting with a commercial mapper, we built a mapping system which uses a two-channel (measurement + reference) mapper probe. We used this system to map and then to shim two magnets of Florida Bitter type at the National High Magnetic Field Laboratory in Tallahassee, FL. With a combination of passive (ferromagnetic) and active shims we achieved 2.3 ppm homogeneity in 1 cm diameter spherical volume (dsv) at 25.0 T in the Keck resistive magnet, and 0.9 ppm homogeneity in 1 cm dsv at 23.5, 28.2, and 35.2 T in the series-connected resistive-superconductive hybrid (SCH) magnet.

Reduction of magnetic field fluctuations in powered magnets for NMR using inductive measurements and sampled-data feedback control.

Resistive and hybrid (resistive/superconducting) magnets provide substantially higher magnetic fields than those available in low-temperature superconducting magnets, but their relatively low spatial homogeneity and temporal field fluctuations are unacceptable for high resolution NMR. While several techniques for reducing temporal fluctuations have demonstrated varying degrees of success, this paper restricts attention to methods that utilize inductive measurements and feedback control to actively cancel the temporal fluctuations. In comparison to earlier studies using analog proportional control, this paper shows that shaping the controller frequency response results in significantly higher reductions in temporal fluctuations. Measurements of temporal fluctuation spectra and the frequency response of the instrumentation that cancels the temporal fluctuations guide the controller design. In particular, we describe a sampled-data phase-lead-lag controller that utilizes the internal model principle to selectively attenuate magnetic field fluctuations caused by the power supply ripple. We present a quantitative comparison of the attenuation in temporal fluctuations afforded by the new design and a proportional control design. Metrics for comparison include measurements of the temporal fluctuations using Faraday induction and observations of the effect that the fluctuations have on nuclear resonance measurements.

The structural topology of wild-type phospholamban in oriented lipid bilayers using 15N solid-state NMR spectroscopy.

For the first time, 15N solid-state NMR experiments were conducted on wild-type phospholamban (WT-PLB) embedded inside mechanically oriented phospholipid bilayers to investigate the topology of its cytoplasmic and transmembrane domains. 15N solid-state NMR spectra of site-specific 15N-labeled WT-PLB indicate that the transmembrane domain has a tilt angle of 13 degrees+/-6 degrees with respect to the POPC (1-palmitoyl-2-oleoyl-sn-glycero-phosphocholine) bilayer normal and that the cytoplasmic domain of WT-PLB lies on the surface of the phospholipid bilayers. Comparable results were obtained from site-specific 15N-labeled WT-PLB embedded inside DOPC/DOPE (1,2-dioleoyl-sn-glycero-3-phosphocholine/1,2-dioleoyl-sn-glycero-3-phosphoethanolamine) mechanically oriented phospholipids' bilayers. The new NMR data support a pinwheel geometry of WT-PLB, but disagree with a bellflower structure in micelles, and indicate that the orientation of the cytoplasmic domain of the WT-PLB is similar to that reported for the monomeric AFA-PLB mutant.