Title: Automated thermal extraction-desorption gas chromatography mass spectrometry: A multifunctional tool for comprehensive characterization of polymers and their degradation products

Abstract

The TED-GC–MS analysis is a two-step method. A sample is first decomposed in a thermogravimetric analyzer (TGA) and the gaseous decomposition products are then trapped on a solid-phase adsorber. Subsequently, the solid-phase adsorber is analyzed with thermal desorption gas chromatography mass spectrometry (TDU-GC–MS). This method is ideally suited for the analysis of polymers and their degradation processes. A new entirely automated system is introduced which enables high sample throughput and reproducible automated fractioned collection of decomposition products. The fractionated collection together with low temperatures reduces the risk of contamination, improves instrumental stability and minimizes maintenance efforts. Through variation of the two main parameters (purge gas flow and heating rate) it is shown how the extraction process can be optimized. By measuring the decomposition products of polyethylene it is demonstrated that compounds with masses of up to 434 Da can be detected. This is achieved despite the low temperature (˜40 °C) of the solid-phase adsorber and the low thermal desorption temperature of 200 °C in the TDU unit. It is now shown that automated TED-GC–MS represents a new flexible multi-functional method for comprehensive polymer analyses. Comparable polymer characterization was previously only achievable through a combination of multiple independent analytical methods. Thismore » is demonstrated by three examples focused on practical challenges in materials analysis and identification: The first one is the analysis of wood plastic composites for which the decomposition processes of the polymer and the bio polymer (wood) could be clearly distinguished by fractionated collection using sequential adsorbers. Secondly, a fast quantitative application is shown by determining the weight concentrations of an unknown polyolefin blend through comparison with a reference material. Additionally, the determination of microplastic concentrations in environmental samples is becoming an increasingly important analytical necessity. It is demonstrated that with TED-GC–MS calibration curves showing good linearity for the most important precursors for microplastic, even complex matrix materials (suspended particulate matter) can be successfully analyzed.« less

Authors:

Duemichen, E. ^[1]; Eisentraut, P. ^[1]; Celina, M. ^[2]; Braun, U. ^[1]

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+ Show Author Affiliations

1. Federal Inst. for Materials Research and Testing (BAM), Berlin (Germany)
2. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Organic Materials Science Dept.

Publication Date:

Fri Jan 11 00:00:00 EST 2019

Research Org.:

Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Federal Inst. for Materials Research and Testing (BAM), Berlin (Germany)

Sponsoring Org.:

USDOE National Nuclear Security Administration (NNSA); German Federal Ministry of Education and Research (BMBF)

OSTI Identifier:

1492387

Report Number(s):

SAND-2018-10731J
Journal ID: ISSN 0021-9673; 668263

Grant/Contract Number:  

NA0003525; 02WRS1378A

Resource Type:

Accepted Manuscript

Journal Name:

Journal of Chromatography

Additional Journal Information:

Journal Volume: 1592; Journal ID: ISSN 0021-9673

Publisher:

Elsevier

Country of Publication:

United States

Language:

English

Subject:

36 MATERIALS SCIENCE; polymer analysis; degradation; thermal desorption; solid-phase adsorber; identification of microplastics; TED-GC–MS