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Use of steady state free precession (SSFP) to enhance signal to noise ratio in high resolution NMR

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Author(s):
Poliana Macedo dos Santos
Total Authors: 1
Document type: Master's Dissertation
Press: São Carlos.
Institution: Universidade de São Paulo (USP). Instituto de Química de São Carlos (IQSC/BT)
Defense date:
Examining board members:
Luiz Alberto Colnago; Roberto Gomes de Souza Berlinck; Antonio Gilberto Ferreira
Advisor: Luiz Alberto Colnago
Abstract

It was performed a detailed analysis of the advantages and disadvantages of Steady State Free Precession (SSFP) sequence for a rapid acquisition of 13C Nuclear Magnetic Resonance (NMR) spectra. The SSFP regime is obtained by the application of a pulse train with the same phase, duration and intensity, separated by a time interval (Tp) shorter than the transverse (T2) and longitudinal (T1) relaxation times. In these conditions it is possible to accumulate tens of spectra per units of T1, providing a significant increase in the spectrum signal-to-noise ratio (s/n). By comparing the spectra obtained by SSFP and conventional pulse sequence (90 degree pulse and T 5T1 p >= ) it was noted that SSFP shows an average gain of 30 times in analysis time for the same s/n. However, the SSFP spectra show phase and intensity anomalies due to the refocusing of the magnetization, generating a spin echo. We also compared the SSFP with the standard 13C pulse sequence, that uses a 30 degree pulses and Tp = 1.38 s. In this comparison the SSFP gain were small (5,5 times in analysis time for the same s/n), because the standard sequence also uses the advantage of SSFP (Tp < T1, T2). The echo signal and the phase anomalies are not observed in the standard sequence because the signal acquisition is truncated at 0.9s and the cycling of the pulse phase, that partially destroy the SSFP coherence. We also analyzed the methods proposed by Rudakov, Freeman and Hill and Schwenk to suppress those anomalies in the 13C NMR spectrum when acquired in SSFP regime. The results showed that the application of these methodologies provides a significant improvement in the spectrum quality. However, it was verified that none of the methods were able to completely eliminate the phase and intensity anomalies. (AU)