Maximising the sharing of the Nottingham DNP MAS NMR Facility

诺丁汉DNP MAS设施是通过物理、化学和生命科学学院联合提交的EPSRC战略设备申请于2015年建立的。自该机制实施以来，可以通过两种不同的途径进入该机制。按成本计算的接入需要支付FEC运营费用(GB 1k/天)，并实施了一条免费接入路线，以允许用户运行可行性和情节项目。中试和可行性研究对DNP MAS核磁共振特别重要，因为这种方法提供的灵敏度增益关键取决于样品制备的优化。通过成本路线进入的时间百分比从最初的2%增加到第二年的31%，但这不足以在2018年8月底之后可持续地运营该设施，届时EPSRC对免费进入路线的现有资金将耗尽。将EPSRC对运营成本的贡献再延长两年，从而通过使用有针对性的行动增加用户组并增加可行性研究到提交给RCUK的拨款提案的转化，从而最大化设备共享。固体魔角旋转(MAS)核磁共振谱(MAS)与动态核极化(DNP)相结合，最近已成为在原子水平上表征非晶态或非均质材料和生物系统的结构和动力学的一种强大技术。相对于传统的固态核磁共振，较大的灵敏度增益允许进行目前因时间限制而不可行的实验。例如，在低自然丰度(例如17O)下检测不敏感的同位素，以及在成对的原子核(例如13C或15N)之间进行关联实验。此外，首次可以检测到吸附在表面的分子或完整细胞中的蛋白质发出的核磁共振信号。DNP的基础是使用强微波场将显著更大的电子自旋极化从顺磁中心转移到感兴趣的核自旋。成功的一个关键步骤是最佳的样品制备，在该样品制备中，被研究的材料与有机自由基混合。DNP MAS核磁共振的巨大潜力导致了最近一波研究活动的激增，目的是更详细地了解DNP的基础物理，并优化样品制备的实验方案。

The Nottingham DNP MAS Facility was established in 2015 via an EPSRC strategic equipment application jointly submitted by the Schools of Physics, Chemistry and Life Sciences. Since its implementation access to the Facility could be gained through two different routes. Costed access required the payment of the FEC operating costs (£1k/day) and a free access route was implemented to allow users to run feasibility and plot projects. Pilot and feasibility studies are particularly important for DNP MAS NMR because the sensitivity gain provided by this method crucially depend on the optimization of the sample preparation. The percentage of access time through the costed route has increased from initially 2% to 31% in the second year, but this is not enough to operate the Facility sustainably after the end of August 2018 when current EPSRC funding for the free access route will run out. A case is made to extent the EPSRC contribution to the operating costs for another two years, so that equipment sharing can be maximised by increasing the user group using targeted actions and increasing the conversion of feasibility studies into grant proposals submitted to RCUK.Solid-state magic angle spinning (MAS) NMR spectroscopy in combination with Dynamic Nuclear Polarization (DNP) has recently emerged as a powerful technique for characterizing the structure and dynamics of amorphous or heterogeneous materials and biological systems at the atomic level. The large sensitivity gain relative to conventional solid-state NMR allows experiments to be performed that are currently not feasible because of time constraints. Examples include the detection of insensitive isotopes at low natural abundance (such as 17O) and correlation experiments between pairs of nuclei (such as 13C or 15N). In addition NMR signals from molecules absorbed on surfaces or from proteins in intact cells can be detected for the first time. DNP is based on the transfer of the significantly larger electron spin polarisation from paramagnetic centres to the nuclear spins of interest using a strong microwave field. A critical step for success is the optimal sample preparation in which the material under investigation is mixed with organic radicals. The huge potential of DNP MAS NMR has led to a recent surge of research activity aimed at gaining a more detailed understanding of the underpinning physics of DNP and optimizing experimental protocols for sample preparation.