Analysis of Hydroperoxides in Solid Polyethylene by MAS (13)C NMR and EPR

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{sup 13}C-enriched polyethylene was subjected to {gamma}-irradiation in the presence of air at 25 and 80 C for total doses ranging from 71 to 355 kGy. Significant quantities of hydroperoxides were detected in the 25 C irradiated sample by {sup 13}C magic angle spinning NMR spectroscopy. This method of detection was performed on the solid polymer and required no chemical derivatization or addition of solvent. The chemical stability and subsequent products of the hydroperoxide species were studied by annealing the irradiated samples in air at temperatures ranging from 22 to 110 C. A time-temperature superposition analysis provided an activation energy ... continued below

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25 p.

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ASSINK,ROGER A.; CELINA,MATHIAS C.; DUNBAR,TIMOTHY D.; ALAM,TODD M.; CLOUGH,ROGER LEE & GILLEN,KENNETH T. November 19, 1999.

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  • Sandia National Laboratories
    Publisher Info: Sandia National Labs., Albuquerque, NM, and Livermore, CA
    Place of Publication: Albuquerque, New Mexico

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{sup 13}C-enriched polyethylene was subjected to {gamma}-irradiation in the presence of air at 25 and 80 C for total doses ranging from 71 to 355 kGy. Significant quantities of hydroperoxides were detected in the 25 C irradiated sample by {sup 13}C magic angle spinning NMR spectroscopy. This method of detection was performed on the solid polymer and required no chemical derivatization or addition of solvent. The chemical stability and subsequent products of the hydroperoxide species were studied by annealing the irradiated samples in air at temperatures ranging from 22 to 110 C. A time-temperature superposition analysis provided an activation energy of 108 kJ/mol for the hydroperoxide decomposition process. The primary products of hydroperoxide decomposition were ketones and secondary alcohols with lesser amounts of acids and esters. EPR measurements suggest that the reactive hydroperoxide species reside in the amorphous phase of polyethylene, consistent with degradation occurring in the amorphous phase.

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25 p.

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INIS; OSTI as DE00014831

Medium: P; Size: 25 pages

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  • Journal Name: Macromolecules; Other Information: Submitted to Macromolecules

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  • Report No.: SAND99-2988J
  • Grant Number: AC04-94AL85000
  • Office of Scientific & Technical Information Report Number: 14831
  • Archival Resource Key: ark:/67531/metadc620362

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Reports, articles and other documents harvested from the Office of Scientific and Technical Information.

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  • November 19, 1999

Added to The UNT Digital Library

  • June 16, 2015, 7:43 a.m.

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  • April 10, 2017, 6:05 p.m.

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ASSINK,ROGER A.; CELINA,MATHIAS C.; DUNBAR,TIMOTHY D.; ALAM,TODD M.; CLOUGH,ROGER LEE & GILLEN,KENNETH T. Analysis of Hydroperoxides in Solid Polyethylene by MAS (13)C NMR and EPR, article, November 19, 1999; Albuquerque, New Mexico. (digital.library.unt.edu/ark:/67531/metadc620362/: accessed December 15, 2018), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.