Institute of Physical and Theoretical Chemistry and Center of Biomolecular Magnetic Resonance, Goethe University Frankfurt, Germany.
Phys Chem Chem Phys. 2010 Jun 14;12(22):5786-90. doi: 10.1039/c003697h. Epub 2010 May 11.
Dynamic nuclear polarization (DNP) at high magnetic fields (9.2 T, 400 MHz (1)H NMR frequency) requires high microwave power sources to achieve saturation of the EPR transitions. Here we describe the first high-field liquid-state DNP results using a high-power gyrotron microwave source (20 W at 260 GHz). A DNP enhancement of -29 on water protons was obtained for an aqueous solution of Fremy's Salt; in comparison the previous highest value was -10 using a solid-state microwave power source (maximum power 45 mW). The increased enhancements are partly due to larger microwave saturation and elevated sample temperature. These experimentally observed DNP enhancements, which by far exceed the predicted values extrapolated from low-field DNP experiments, demonstrate experimentally that DNP is possible in the liquid state also at high magnetic fields.
在高磁场(9.2T,400MHz(1)H NMR 频率)下进行动态核极化(DNP)需要高功率微波源来实现电子顺磁共振跃迁的饱和。在这里,我们描述了使用高功率回旋管微波源(260GHz 时 20W)的第一个高场液相 DNP 结果。对于 Fremy 盐的水溶液,获得了水质子的 DNP 增强-29;相比之下,以前使用固态微波功率源(最大功率 45mW)获得的最高值为-10。增强部分归因于更大的微波饱和和升高的样品温度。这些实验观察到的 DNP 增强值远远超过从低场 DNP 实验外推的预测值,从实验上证明了在高磁场下也可以在液相中进行 DNP。