利用 ATR-FTIR 分析氟橡胶化合物的特性

Christine Rabello Nascimento, Daniele Rosendo de Lima, Janaina Fernandes Moreno de Almeida, Ana Maria Furtado de Sousa, Cristiane Xavier da Silva Campos, Fernando Reis da Cunha, Ana Lúcia Nazareth da Silva
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摘要

氟橡胶 (FKM) 用于制造密封件和其他橡胶装置,可承受恶劣的工作条件,包括侵蚀性介质和极端的低温和高温。尽管核磁共振、傅立叶变换红外光谱(FTIR)和色谱技术已被广泛用于表征未加工的 FKM 分子,但要识别固化化合物,还需要一种能够克服与此类结构相关的复杂性的表征方法。从这个意义上说,衰减全反射傅立叶变换红外(ATR-FTIR)光谱法无需溶解或对样品进行任何特殊制备,因此优于其他表征技术。本研究利用四种商用 FKM 和填充剂炭黑、硫酸钡和氧化铁生产了 10 种 FKM 复合物。所有未填充的 FKM(原样)及其化合物都用锗晶体进行了 ATR-FTIR 分析。对每种 FKM 样品及其化合物进行了 15 至 25 次分析。对所有光谱进行了分析,并对条带进行了分配。此外,还报告了填料对光谱的干扰情况。根据光谱带的高度与 1397 和 1428 cm-1 处的光谱带之间的关系,可以区分 FKM 类型 1、2、3 和 5 的所有样品成分。这项研究表明,ATR-傅立叶变换红外光谱技术具有检测 FKM 化合物类型的潜力,FKM 是一种重要的橡胶,可用于苛刻的工业应用中。用 BaSO4 替代碳可降低 FKM 类型 1 和 2 复合材料在 50% 应变时的拉伸强度。填充了 30 phr 碳黑的 FKM 类型 3 和 5 复合材料在 50%应变时的拉伸强度高于 FKM 类型 1 的复合材料。
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Characterization of fluoroelastomers compounds by ATR-FTIR
Fluoroelastomers (FKM) are used to manufacture seals and other rubber devices that can withstand harsh operating conditions, including aggressive media and extreme low and high temperatures. Even though nuclear magnetic resonance, Fourier-transform infrared spectroscopy (FTIR), and chromatographic techniques have been extensively used in the characterization of raw FKM molecules, the identification of cured compounds entails a characterization method that is able to overcome the complexity related to this kind of structure. In this sense, attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy can outperform other characterization techniques because it does not require solubilization or any special preparation of the sample. In this study, 10 FKM compounds were produced in this study utilizing four commercial types of FKM and the fillers carbon black, barium sulfate, and iron oxide. All unfilled-FKM (as received) and their compounds were analyzed by ATR-FTIR with germanium crystal. Between 15 and 25 analyses were performed for all each FKM type sample and their respective compounds. All spectra were analyzed, and the bands were assigned. Findings regarding the interference of the fillers in the spectra were also reported. From relationships between the height of the spectral zones and the bands at 1397 and 1428 cm−1, it was possible to distinguish all sample compositions of FKM types 1, 2, 3, and 5. This study demonstrates that ATR-FTIR has the potential to be utilized as a technique to detect the type of FKM compounds, an important rubber used in harsh industrial applications. Replacing carbon with BaSO4 reduces the tensile at 50% strain of FKM types 1 and 2 composites. FKM types 3 and 5 composites filled with 30 phr of carbon black have a higher tensile at 50% strain than those of FKM type 1.
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