Isolation and monitoring of the endohedral metallofullerenes YC{sub 82} and Sc{sub 3}C{sub 82}. On-line chromatographic separation with EPR detection
- Virginia Polytechnic Inst. and State Univ., Blacksburg, VA (United States)
- California Inst. of Technology, Pasadena, CA (United States)
- IBM Research Division, San Jose, CA (United States)
The direct coupling of high-performance liquid chromatography (HPLC) with on-line electron paramagnetic resonance (EPR) detection is demonstrated for monitoring separations of endohedral metallofullerenes (MC{sub 2a}). The HPLC-EPR approach readily permits detection of the paramagnetic species, such as YC{sub 82} and Sc{sub 3}C{sub 82}, in the presence of the dominant empty-cage fullerenes (C{sub 60}, C{sub 70}) and diamagnetic metallofullerenes (e.g., M{sub 2}C{sub 2n}). The results indicate that on-line EPR provides a noninvasive, selective detector for HPLC metallofullerene separations that is readily adaptable to air-sensitive and/or labile compounds. Specifically, the `EPR-active` metallofullerenes, YC{sub 82} and Sc{sub 3}C{sub 82}, are selectively monitored on-line for an initial separation of the metallofullerene fraction from the dominant empty-cage fullerenes utilizing a combination of polystyrene columns. This preparative `cleanup` procedure is followed by HPLC-EPR separation and monitoring of YC{sub 82} and Sc{sub 3}C{sub 82} species using a selective tripodal {pi}-acidic-phase column (Trident-Tri-DNP) for the final stages of isolation. 30 refs., 8 figs.
- Sponsoring Organization:
- USDOE
- OSTI ID:
- 102756
- Journal Information:
- Analytical Chemistry (Washington), Journal Name: Analytical Chemistry (Washington) Journal Issue: 17 Vol. 66; ISSN 0003-2700; ISSN ANCHAM
- Country of Publication:
- United States
- Language:
- English
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