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Title: High temperature polymer degradation: Rapid IR flow-through method for volatile quantification

Accelerated aging of polymers at elevated temperatures often involves the generation of volatiles. These can be formed as the products of oxidative degradation reactions or intrinsic pyrolytic decomposition as part of polymer scission reactions. A simple analytical method for the quantification of water, CO 2, and CO as fundamental signatures of degradation kinetics is required. Here, we describe an analytical framework and develops a rapid mid-IR based gas analysis methodology to quantify volatiles that are contained in small ampoules after aging exposures. The approach requires identification of unique spectral signatures, systematic calibration with known concentrations of volatiles, and a rapid acquisition FTIR spectrometer for time resolved successive spectra. Furthermore, the volatiles are flushed out from the ampoule with dry N2 carrier gas and are then quantified through spectral and time integration. This method is sufficiently sensitive to determine absolute yields of ~50 μg water or CO 2, which relates to probing mass losses of less than 0.01% for a 1 g sample, i.e. the early stages in the degradation process. Such quantitative gas analysis is not easily achieved with other approaches. Our approach opens up the possibility of quantitative monitoring of volatile evolution as an avenue to explore polymer degradationmore » kinetics and its dependence on time and temperature.« less
Authors:
 [1] ;  [1]
  1. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Organic Materials Science Dept.
Publication Date:
Report Number(s):
SAND-2017-5314J; SAND2017-5314J
Journal ID: ISSN 0141-3910; PII: S0141391017301362
Grant/Contract Number:
AC04-94AL85000
Type:
Accepted Manuscript
Journal Name:
Polymer Degradation and Stability
Additional Journal Information:
Journal Volume: 145; Journal ID: ISSN 0141-3910
Publisher:
Elsevier
Research Org:
Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
Sponsoring Org:
USDOE National Nuclear Security Administration (NNSA)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; Accelerated aging; Thermo-sets; Thermal stability; IR gas spectroscopy; Volatile analysis; Off-gassing quantification
OSTI Identifier:
1360931
Alternate Identifier(s):
OSTI ID: 1464176

Giron, Nicholas H., and Celina, Mathew C.. High temperature polymer degradation: Rapid IR flow-through method for volatile quantification. United States: N. p., Web. doi:10.1016/j.polymdegradstab.2017.05.013.
Giron, Nicholas H., & Celina, Mathew C.. High temperature polymer degradation: Rapid IR flow-through method for volatile quantification. United States. doi:10.1016/j.polymdegradstab.2017.05.013.
Giron, Nicholas H., and Celina, Mathew C.. 2017. "High temperature polymer degradation: Rapid IR flow-through method for volatile quantification". United States. doi:10.1016/j.polymdegradstab.2017.05.013. https://www.osti.gov/servlets/purl/1360931.
@article{osti_1360931,
title = {High temperature polymer degradation: Rapid IR flow-through method for volatile quantification},
author = {Giron, Nicholas H. and Celina, Mathew C.},
abstractNote = {Accelerated aging of polymers at elevated temperatures often involves the generation of volatiles. These can be formed as the products of oxidative degradation reactions or intrinsic pyrolytic decomposition as part of polymer scission reactions. A simple analytical method for the quantification of water, CO2, and CO as fundamental signatures of degradation kinetics is required. Here, we describe an analytical framework and develops a rapid mid-IR based gas analysis methodology to quantify volatiles that are contained in small ampoules after aging exposures. The approach requires identification of unique spectral signatures, systematic calibration with known concentrations of volatiles, and a rapid acquisition FTIR spectrometer for time resolved successive spectra. Furthermore, the volatiles are flushed out from the ampoule with dry N2 carrier gas and are then quantified through spectral and time integration. This method is sufficiently sensitive to determine absolute yields of ~50 μg water or CO2, which relates to probing mass losses of less than 0.01% for a 1 g sample, i.e. the early stages in the degradation process. Such quantitative gas analysis is not easily achieved with other approaches. Our approach opens up the possibility of quantitative monitoring of volatile evolution as an avenue to explore polymer degradation kinetics and its dependence on time and temperature.},
doi = {10.1016/j.polymdegradstab.2017.05.013},
journal = {Polymer Degradation and Stability},
number = ,
volume = 145,
place = {United States},
year = {2017},
month = {5}
}