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

Giron, Nicholas H.; Celina, Mathew C.

doi:10.1016/j.polymdegradstab.2017.05.013

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

Journal Article · Fri May 19 00:00:00 EDT 2017 · Polymer Degradation and Stability

DOI:https://doi.org/10.1016/j.polymdegradstab.2017.05.013· OSTI ID:1360931

Giron, Nicholas H. ^[1]; Celina, Mathew C. ^[1]

Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Organic Materials Science Dept.

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.

View Accepted Manuscript (DOE)

Research Organization:: Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)

Sponsoring Organization:: USDOE National Nuclear Security Administration (NNSA)

Grant/Contract Number:: AC04-94AL85000

OSTI ID:: 1360931

Alternate ID(s):: OSTI ID: 1550080
OSTI ID: 1464176

Report Number(s):: SAND--2017-5314J; PII: S0141391017301362

Journal Information:: Polymer Degradation and Stability, Journal Name: Polymer Degradation and Stability Vol. 145; ISSN 0141-3910

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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