Removing acoustic ringing baseline curvature in 13C NMR spectra for quantitative analyses

• Published in: Magnetic resonance in chemistry Vol. 61; no. 9-10; pp. 544 - 553
• Main Authors: Vasquez, Joseph K, Zhou, Zhe, Clark, Brian, Kimenai, Ad J, Reiner, Benjamin R, Rau, Nathan J, Baugh, Dan, Eldred, Donald V, Paradkar, Manjiri, Chen, Zheng, DeFelippis, Jim, Potter, Janece M, Qiu, Xiao Hua, Zong, Xiaohong, Wenshiue Owen Young, Fitzgibbons, Thomas, Moreno, Aitor, Freudenberger, Christoph, Mayzel, Maksim
• Format: Journal Article
• Language: English
• Published: Bognor Regis Wiley Subscription Services, Inc 01.09.2023
• Subjects: Broadband; Cryoprobes; Curvature; NMR; Nuclear magnetic resonance; Process parameters; Quantitative analysis; Spectra; Spectrometers
• ISSN: 0749-1581; 1097-458X
• DOI: 10.1002/mrc.5384

13C nuclear magnetic resonance (NMR) is traditionally considered an insensitive technique, requiring long acquisition times to measure dilute functionalities on large polymers. With the introduction of cryoprobes and better electronics, sensitivity has improved in a way that allows measurements to take less than 1/20th the time that they previously did. Unfortunately, a high Q‐factor with cryoprobes creates baseline curvature related to acoustic ringing that affects quantitative NMR analyses. Manual baseline correction is commonly used to compensate for the baseline roll, but it is a time‐intensive process. The outcome of manual baseline correction can vary depending on processing parameters, especially for complicated spectra. Additionally, it can be challenging to distinguish between broad peaks and baseline rolls. A new anti‐ring pulse sequence (zgig_pisp) was previously reported to improve on the incumbent single pulse experiment (zgig). The original report presented limited comparison data with 13C NMR, but a thorough validation is needed before broader implementation can be considered. In this work, we report the round‐robin testing and comparison of zgig_pisp and zgig pulse sequences. During the testing phase, we found that zgig_pisp is practically equivalent to zgig to ±2% for the majority of integrals examined. Additionally, a short broadband inversion pulse (BIP) was demonstrated as an alternative to the originally reported adiabatic CHIRP shaped pulse. The zgig_pisp pulse sequence code for Bruker spectrometers is also simplified.