A Round-Robin Study on Decomposition of Calcium Oxalate Monohydrate by Thermogravimetry

Published

August 1, 2022

Author(s)

Mathieu Suzanne, Serge Bourbigot, Eric Coker, Loic Dumazert, Talal Fateh, Tuula Hakkarainen, Pedro Lazaro-Urrutia, Isaac Leventon, Guillermo Rein, Franz Richter, Aleksi Rinta-Paavola, Thomas Rogaume, Stanislav Stoliarov, Aurelien Thiry, Artur Witkowski

Abstract

A round-robin study for thermogravimetric analysis (TGA) of carbon oxalate monohydrate was organised with thirteen participants. The main objectives were to provide best practice in the use of TGA and guidelines on uncertainties in the context of pyrolysis and fire modelling. The material studied, calcium oxalate monohydrate, is often used to evaluate the proper functioning of a given piece of equipment because its decomposition steps are well documented and known to be repeatable and reproducible. The experimental procedure was described in as much detail as possible, bearing in mind that it cannot be fully prescribed due to the different technologies of thermogravimetric analysers. All thermograms were evaluated for mass losses and onset, peak and end-set temperatures for the three decomposition steps using two outlier detection methods, the Grubbs method and an alternative two-step method inspired from Z-score technique, allowing an assessment of measurement deviation calculated throughout the duration of the experiment. This study allows a benchmarking of data scatter due to instrument and operator. It confirms that verification with calcium oxalate is a good screening method that can be used by laboratories. Within a laboratory, it can also help to identify problems with instrument accuracy that would otherwise be difficult to detect. This, together with the good practice outlined in the paper, should help the community to increase the validity of tests on other materials of interest to fire science.

Citation

Fire Technology

Pub Type

Journals

Download Paper

https://doi.org/10.1007/s10694-026-01873-8

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Keywords

Round-robin test · Thermogravimetry analysis · Calcium oxalate monohydrate · Thermal decomposition

Citation

Suzanne, M. , Bourbigot, S. , Coker, E. , Dumazert, L. , Fateh, T. , Hakkarainen, T. , Lazaro-Urrutia, P. , Leventon, I. , Rein, G. , Richter, F. , Rinta-Paavola, A. , Rogaume, T. , Stoliarov, S. , Thiry, A. and Witkowski, A. (2022), A Round-Robin Study on Decomposition of Calcium Oxalate Monohydrate by Thermogravimetry, Fire Technology, [online], https://doi.org/10.1007/s10694-026-01873-8, https://tsapps.nist.gov/publication/get_pdf.cfm?pub_id=935144 (Accessed October 20, 2026)

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