Combining Thermogravimetry-Mass Spectrometry and Target Factor Analysis for Rapid Characterization of Volatiles from Degradation of Epoxy Paint

IF 4.1 Q2 CHEMISTRY, ANALYTICAL Analytical science advances Pub Date : 2024-12-07 DOI:10.1002/ansa.202400047
Subhamoy Saha, Ajit N. Shirsat, V. S. Tripathi, Salil Varma, Mathi Pandiyathuray
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Abstract

Thermogravimetry coupled with simultaneous evolved gas analysis by mass spectrometry was used for discerning organic compounds released during the thermal degradation of paint whose chemical compositions are not readily accessible. Thermogravimetric analyses up to 600°C revealed distinct degradation patterns under inert and oxidative conditions. Significant degradation of paint initiates at around 360°C and concludes at 500°C in a nitrogen atmosphere. However, under oxidative conditions, degradation began at 100°C, with notable mass loss extending from 300 to 600°C, with a distinct event at 500°C. Moreover, the overall mass loss in air has been observed to be 3% higher than that in nitrogen. The rapid characterization of the volatiles was made possible by model-free target factor analyses of evolved gas mass spectra. The temperature-correlated mass analyses revealed potential volatile sources, including structural breakdown and oxidative conversion. Comparative analyses revealed predominantly oxidative conversion of organics to CO2 during degradation in air. The evolution of several classes of organics during the thermal degradation of paint is a matter of great concern for postulated accident scenarios in nuclear power plants. The low molecular weight organic volatiles may be taken up by iodine aerosols released into the containment during an accident, potentially forming organic iodides, which are biological hazards. Thus, identifying these volatile organics is crucial for accurately estimating the source term of volatile organic iodine.

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结合热重-质谱和目标因子分析快速表征环氧涂料降解挥发物。
采用热重法结合质谱法对油漆热降解过程中释放的化学成分不易获得的有机化合物进行了分析。热重分析高达600°C,在惰性和氧化条件下显示出明显的降解模式。在氮气气氛中,油漆的显著降解始于360°C左右,并在500°C时结束。然而,在氧化条件下,降解始于100°C,从300°C到600°C有明显的质量损失,在500°C有明显的事件。此外,据观察,空气中的总质量损失比氮中的总质量损失高3%。通过对演化的气体质谱进行无模型目标因子分析,可以快速表征挥发物。温度相关质量分析揭示了潜在的挥发源,包括结构分解和氧化转化。对比分析显示,有机物在空气降解过程中主要是氧化转化为二氧化碳。涂料热降解过程中几类有机物的演变是核电站假想事故情景中非常值得关注的问题。事故发生时,低分子量有机挥发物可能被释放到安全壳内的碘气溶胶吸收,可能形成具有生物危害性的有机碘化物。因此,识别这些挥发性有机物对于准确估计挥发性有机碘的来源项至关重要。
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