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Published on: November 11, 2013
Nondestructive Quantitative Analysis of Lithium Ion-Endohedral Fullerene Salt (Li+@C60·PF6 -) via 19F NMR
Eunsang Kwon1, Shin-Ichiro Yoshida1, Kazuhiko Kawachi2
1Research and Analytical Center for Giant Molecules, Graduate School of Science, Tohoku University, Sendai, Miyagi 980-8578, Japan.
Abstract:
A quantitative analysis of the lithium ion-endohedral fullerene salt, Li+@C60·PF6 - (1), was performed using 19F nuclear magnetic resonance (NMR) spectroscopy. To establish a robust quantitative 19F NMR (qNMR) method, experimental parametersincluding spin-lattice relaxation time (T 1), relaxation delay, and offset frequencywere optimized using tetrabutylammonium hexafluorophosphate (TBA+·PF6 -) as a model compound and α,α,α-trifluorotoluene (PhCF3) as an internal standard. The purity of 1 was determined using a calibration curve constructed from 19F NMR measurements, which effectively minimized systematic errors. The purity value obtained via this nondestructive qNMR method was approximately 95%, showing excellent agreement with quantitative results obtained from inductively coupled plasma atomic emission spectroscopy (95.1%). This method offers a rapid, specific, and nondestructive alternative for the purity evaluation of endohedral metallofullerenes allowing for complete sample recovery.
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