波谱学杂志
波譜學雜誌
파보학잡지
CHINESE JOURNAL OF MAGNETIC RESONANCE
2015年
2期
363-372
,共10页
郑人豪%吴振%黄柏绮%柯志正%丁尚武
鄭人豪%吳振%黃柏綺%柯誌正%丁尚武
정인호%오진%황백기%가지정%정상무
固体核磁共振%四极核%多量子跃迁魔角旋转%卫星跃迁魔角旋转%脉冲优化
固體覈磁共振%四極覈%多量子躍遷魔角鏇轉%衛星躍遷魔角鏇轉%脈遲優化
고체핵자공진%사겁핵%다양자약천마각선전%위성약천마각선전%맥충우화
solid-state NMR%quadrupolar nuclei%MQMAS%STMAS%pulse optimization
该文提出一个能使多量子跃迁、卫星跃迁魔角旋转及其变种方法的灵敏度明显增强的方法.在通常多量子激发或卫星跃迁激发脉冲之前施加一个预备脉冲,对初始态优化从而使循环延迟时间显著减小.利用几个代表性核种(23Na,11B和87Rb)在两个不同磁场下演示了这一方法.该方法可在低至4.7 T的磁场及6 kHz的转速下在任何常规固体核磁共振实验中实现,无需附加硬件或软件.此外,尽管完整的理论解说将另行发表,文中给出具体的实验步骤,使该方法可由用户灵活订制实验,针对每个样品优化实验参数.
該文提齣一箇能使多量子躍遷、衛星躍遷魔角鏇轉及其變種方法的靈敏度明顯增彊的方法.在通常多量子激髮或衛星躍遷激髮脈遲之前施加一箇預備脈遲,對初始態優化從而使循環延遲時間顯著減小.利用幾箇代錶性覈種(23Na,11B和87Rb)在兩箇不同磁場下縯示瞭這一方法.該方法可在低至4.7 T的磁場及6 kHz的轉速下在任何常規固體覈磁共振實驗中實現,無需附加硬件或軟件.此外,儘管完整的理論解說將另行髮錶,文中給齣具體的實驗步驟,使該方法可由用戶靈活訂製實驗,針對每箇樣品優化實驗參數.
해문제출일개능사다양자약천、위성약천마각선전급기변충방법적령민도명현증강적방법.재통상다양자격발혹위성약천격발맥충지전시가일개예비맥충,대초시태우화종이사순배연지시간현저감소.이용궤개대표성핵충(23Na,11B화87Rb)재량개불동자장하연시료저일방법.해방법가재저지4.7 T적자장급6 kHz적전속하재임하상규고체핵자공진실험중실현,무수부가경건혹연건.차외,진관완정적이론해설장령행발표,문중급출구체적실험보취,사해방법가유용호령활정제실험,침대매개양품우화실험삼수.
A method to significantly enhance the sensitivity of the widely used multiple quantum magic angle spinning (MQMAS), satellite transition magic angle spinning (STMAS) and their variants is proposed. By introducing a preparatory period prior to the normal multiple quantum excitation or satellite transition pulse, the initial state can be optimized so that the recycle delay time can be substantially reduced. The performance of this method, for both MQMAS and STMAS in two different magnetic fields, has been demonstrated with a number of representative nuclear species (23Na,11B and87Rb). This method can be implemented, without any additional hardware or software accessories, on all conventional solid-state NMR spectrometers with operating magnetic field as low as 4.7 T and sample spinning speed as slow as 6 kHz. Moreover, it is a very flexible method so that it can be customized, i.e., for individual compounds, the experimental parameters can be optimized for each compound following a step-by-step procedure specified in this work although a full theoretical exposition will be provided separately.