Synthesis, characterization, and neutron activation of holmium metallofullerenes
Abstract
Isolation of the first macroscopic quantities of endohedral holmium metallofullerenes (principally Ho@C{sub 82}, Ho{sub 2}@C{sub 82}, and Ho{sub 3}@C{sub 82} by LD-TOF mass spectrometry) has been accomplished by carbon-arc and preparative HPLC methodologies. The detailed procedure for production and isolation of the metallofullerenes includes a new technique whereby holmium-impregnated electrodes are prepared simply by soaking porous graphite rods in an ethanolic solution of Ho(NO{sub 3}){sub 3}.xH{sub 2}O. Monoisotopic {sup 165}Ho offers a unique combination of advantages for neutron-activation studies of metallofullerenes, and purified samples containing {sup 165}Ho@C{sub 82}, {sup 165}Ho{sub 2}@C{sub 82}, and {sup 165}Ho{sub 3}@C{sub 82} have been activated by high-flux neutron irradiation ({Phi} = 4 x 10{sup 13}n cm{sup -2} s{sup -1}) to generate {sup 166}Ho metallofullerenes, which undergo {beta}{sup -} decay to produce stable {sup 166}Er. Chemical workup of the irradiated samples, followed by re-irradiation, has been used to demonstrate that observed decomposition of holmium metallofullerenes is due mainly to `fast` neutron damage rather than to holmium atom nuclear recoil (E{sub max} = 200 eV). This implies that metallofullerene damage can be minimized by using neutron fluxes with the highest possible thermal component. 60 refs., 4 figs.
- Authors:
-
- Rice Univ., Houston, TX (United States)
- TDA Research, Wheat Ridge, CO (United States)
- NanoTechnologies of Texas, Bellaire, TX (United States)
- Univ. of Missouri, Columbia, MO (United States)
- Publication Date:
- OSTI Identifier:
- 380777
- Resource Type:
- Journal Article
- Journal Name:
- Journal of the American Chemical Society
- Additional Journal Information:
- Journal Volume: 118; Journal Issue: 34; Other Information: PBD: 28 Aug 1996
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 36 MATERIALS SCIENCE; 40 CHEMISTRY; HOLMIUM COMPOUNDS; SYNTHESIS; NEUTRON ACTIVATION ANALYSIS; DECOMPOSITION; MASS SPECTRA; FULLERENES; SEPARATION PROCESSES
Citation Formats
Cagle, D W, Thrash, T P, Wilson, L J, Alford, M, Chibante, L P.F., and Ehrhardt, G J. Synthesis, characterization, and neutron activation of holmium metallofullerenes. United States: N. p., 1996.
Web. doi:10.1021/ja960841z.
Cagle, D W, Thrash, T P, Wilson, L J, Alford, M, Chibante, L P.F., & Ehrhardt, G J. Synthesis, characterization, and neutron activation of holmium metallofullerenes. United States. https://doi.org/10.1021/ja960841z
Cagle, D W, Thrash, T P, Wilson, L J, Alford, M, Chibante, L P.F., and Ehrhardt, G J. 1996.
"Synthesis, characterization, and neutron activation of holmium metallofullerenes". United States. https://doi.org/10.1021/ja960841z.
@article{osti_380777,
title = {Synthesis, characterization, and neutron activation of holmium metallofullerenes},
author = {Cagle, D W and Thrash, T P and Wilson, L J and Alford, M and Chibante, L P.F. and Ehrhardt, G J},
abstractNote = {Isolation of the first macroscopic quantities of endohedral holmium metallofullerenes (principally Ho@C{sub 82}, Ho{sub 2}@C{sub 82}, and Ho{sub 3}@C{sub 82} by LD-TOF mass spectrometry) has been accomplished by carbon-arc and preparative HPLC methodologies. The detailed procedure for production and isolation of the metallofullerenes includes a new technique whereby holmium-impregnated electrodes are prepared simply by soaking porous graphite rods in an ethanolic solution of Ho(NO{sub 3}){sub 3}.xH{sub 2}O. Monoisotopic {sup 165}Ho offers a unique combination of advantages for neutron-activation studies of metallofullerenes, and purified samples containing {sup 165}Ho@C{sub 82}, {sup 165}Ho{sub 2}@C{sub 82}, and {sup 165}Ho{sub 3}@C{sub 82} have been activated by high-flux neutron irradiation ({Phi} = 4 x 10{sup 13}n cm{sup -2} s{sup -1}) to generate {sup 166}Ho metallofullerenes, which undergo {beta}{sup -} decay to produce stable {sup 166}Er. Chemical workup of the irradiated samples, followed by re-irradiation, has been used to demonstrate that observed decomposition of holmium metallofullerenes is due mainly to `fast` neutron damage rather than to holmium atom nuclear recoil (E{sub max} = 200 eV). This implies that metallofullerene damage can be minimized by using neutron fluxes with the highest possible thermal component. 60 refs., 4 figs.},
doi = {10.1021/ja960841z},
url = {https://www.osti.gov/biblio/380777},
journal = {Journal of the American Chemical Society},
number = 34,
volume = 118,
place = {United States},
year = {Wed Aug 28 00:00:00 EDT 1996},
month = {Wed Aug 28 00:00:00 EDT 1996}
}