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Title: 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:
; ;  [1];  [2];  [3];  [4]
  1. Rice Univ., Houston, TX (United States)
  2. TDA Research, Wheat Ridge, CO (United States)
  3. NanoTechnologies of Texas, Bellaire, TX (United States)
  4. 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}
}