Analytical Instrument Documents

15N NMR is widely used because of the importance of nitrogen in chemistry, materials, biology, environment, etc. However, very low abundance of 15N (<0.4%) results in poor sensitivity and thus makes observation time-consuming. On the other hand, the rest of nitrogen atoms are also NMR sensitive nucleus of 14N. Despite the high abundance of 14N (>99%), it's application is rather limited due to the huge quadrupolar interactions and its spin quantum number I = 1.

JEOL AUTOMAS probe combined with Auto Sample Changer and Auto Tune Unit allows for fully automated solid NMR measurements including sample load/eject, tuning and matching, magic angle spinning frequency control, and temperature control. This enables you to manage efficient data collection as liquid NMR.

We can supply 2.5, 3.2 or 4.0 mm XY-MAS probes suitable for inorganic materials. The XY-MAS probe has two rf channels which enable simultaneous strong rf-field irradiation.

Here we present the recent development at RIKEN CLST-JEOL collaboration laboratory to explore the molecular structures of low-molecular weight pharmaceutical compounds in natural abundance (without any isotopic labeling); the recent progress in fast magic angle spinning (MAS) technology in solid-state nuclear magnetic resonance (ssNMR) and in ultra high sensitivity camera in transmission electron microscopy (TEM) paves a new way to answer problems in the pharmaceutical industry and sciences. 1) Crystalline polymorphs and 2) salt/cocrystal are two major concerns in terms of quality control, stability, and intellectual property. To identify the crystalline form, powder X-ray diffraction and 13C cross-polarization MAS ssNMR are widely used methods, however, the former is sometimes not suitable for mixture analysis and latter fails to distinguish crystalline forms with similar molecular conformations. To solve these issues, we use electron diffraction (ED) and 1H fast MAS NMR. The crystalline form can be determined from nano- to micro-meter sized single crystals using ED, since electron interactions are 4 to 5 order stronger than X-ray interactions. 1H NMR also gives suitable information to molecular packing since 1H is located at the surface of the crystals. The salt/cocrystal issue, where hydrogen plays a key role, is a serious problem, since single crystal X-ray diffraction (SCXRD) cannot determine the hydrogen atom position precisely. Here we determine the internuclear distances between 1H and 15N using ssNMR at fast MAS conditions, while the global structure is obtained through SCXRD, answering the salt/cocrystal questions.