Solid-state NMR as an analytical tool: quantitative aspects.
Analytical methods based on solid-state NMR are becoming increasingly popular. However, these flourishing activities bring up the issue of how accurately NMR can assess an analyte proportion in a solid sample. The use of a chemical intensity reference for this purpose is a natural but often unsuitable choice, due to sample stability or preciousness. We propose here a protocol to perform quantitative measurements in solid-state NMR, by calibration of the circuit response through a low-power pulse injected during the acquisition (the so-called ERETIC method). Although this method has been in use for some time in liquid-phase and in vivo NMR, we point out here some peculiarities and useful applications typical of solids. Namely, the temperature dependence of the signal intensity imposes care in the application to MAS experiments.
Ziarelli
Fabio
F
Spectropole, Fédération des Sciences Chimiques de Marseille, Campus de Saint Jérôme, 13013 Marseille, France.
Caldarelli
Stefano
S
D002138:Calibration; D009682:Magnetic Resonance Spectroscopy / Q000295:instrumentation* / Q000379:methods* / Q000592:standards; D011208:Powders / Q000032:analysis* / Q000737:chemistry*; D012016:Reference Values; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013696:Temperature
D011208:Powders