1994
DOI: 10.1021/ac00089a014
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Isolation and Monitoring of the Endohedral Metallofullerenes Y@C82 and Sc3@C82: Online Chromatographic Separation with EPR Detection

Abstract: 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 (M a C2n). The HPLC-EPR approach readily permits detection of the paramagnetic species, such as Y @C82 and Sc3@C82, in the presence of the dominant empty-cage fullerenes (C, C70) and diamagnetic metallofullerenes (e.g., M2@Czn). The results indicate that on-line EPR provides a noninvasive, selective detector … Show more

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Cited by 47 publications
(15 citation statements)
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“…To remove the lower mass empty-cage fullerenes (e.g., C 60 , C 70 , and C 84 ), this solution was injected into two polystyrene columns that were connected in series. To obtain the metallofullerene fraction, on-line electron paramagnetic resonance (EPR) detection was implemented as previously described . As previously demonstrated, the EPR-active metallofullerenes (A m @C 2 n , m = 1 or 3) nicely serve as “markers” for the overall coelution of the metallofullerene fraction. , The separation on this polystyrene chromatographic phase was subsequently performed at ambient temperature with a flow rate of 1 mL/min.…”
Section: Resultsmentioning
confidence: 99%
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“…To remove the lower mass empty-cage fullerenes (e.g., C 60 , C 70 , and C 84 ), this solution was injected into two polystyrene columns that were connected in series. To obtain the metallofullerene fraction, on-line electron paramagnetic resonance (EPR) detection was implemented as previously described . As previously demonstrated, the EPR-active metallofullerenes (A m @C 2 n , m = 1 or 3) nicely serve as “markers” for the overall coelution of the metallofullerene fraction. , The separation on this polystyrene chromatographic phase was subsequently performed at ambient temperature with a flow rate of 1 mL/min.…”
Section: Resultsmentioning
confidence: 99%
“…Further details on HPLC instrumentation, on-line EPR detection, and negative-ion mass spectrometry for this study have been previously published. , For the mass spectra obtained from the laser desorption time-of-flight (LD-TOF) method, the wavelength of the ionizing photons used was 193 nm. This mass spectrometry technique enhances the metallofullerene/fullerene ratio since at this wavelength it takes two photons to ionize empty-cage fullerenes, whereas the ionization of the metallofullerenes occurs through only single-photon processes.…”
Section: Methodsmentioning
confidence: 99%
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“…However, the preparation of milligram amounts of endohedral metallofullerenes (∼95% purity) is still very time consuming and solvent consuming and involves multistep chromatographic procedures. This results from a most annoying limiting factor in HPLC separation of endohedral metallofullerenes that in various fullerene solvent extracts empty fullerenes (mainly C 60 and C 70 ) are usually above 2 orders of magnitude more abundant than the endohedral metallofullerenes. One way to circumvent this problem is to improve the HPLC column for higher loading capacity while maintaining a reasonable selectivity .…”
Section: Intrductionmentioning
confidence: 99%
“…One of the spectacular directions of fullerene research involves encapsulation of metal atom(s) inside the fullerene cage to form metal@fullerene endohedral complexes, or metallofullerenes. Since the first observation of metallofullerenes La@C 2 n by Smalley's group in 1985, these exotic molecules have attracted intense interest owing to their unique “super-atom” structures and great application prospects. The utilization of the arc evaporation technique makes it possible to synthesize metallofullerenes in macroscopic quantities, , which can be further purified by HPLC separation. As a result, some studies on their molecular and electronic structures, chemical derivatization, and application have been carried out. …”
Section: Introductionmentioning
confidence: 99%