1H NMR and UV-Vis as Analytical Techniques to Evaluate Biodiesel Conversion and Oxidative Stability

Fuels Pub Date : 2024-03-18 DOI:10.3390/fuels5010007
Emanuelle Braga, Luana Damasceno, Chastryane Barros de Sousa Silva, Lucas Silva, Maria Cavalcante, César Barreto, Silvia Silva, F. M. Luna, Luciana Bertini, Tassio Nascimento, Maria Rios
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Abstract

The present study evaluated the applicability of 1H NMR and UV-Vis spectroscopies as analytical techniques for the characterization and determination of biodiesel conversion and for monitoring the oxidative stability of biodiesel samples with antioxidants. For this study, safflower and babassu biodiesels were obtained through transesterification, and physicochemical properties confirmed the success of both reactions. A bench-top accelerated oxidation system was used as an alternative to the Rancimat® method, with samples of 6.0 g heated at 110 ± 5 °C and collected every 2 h for 12 h. The agreement for biodiesel conversions was good, with divergences between 2% and 0.4% for safflower biodiesel and 1.9% for babassu biodiesel. As for UV-Vis spectroscopy, the technique showed the same trend as the Rancimat® method, showing efficiency in evaluating the oxidative stability of safflower biodiesel and in the performance of antioxidants BHT and DMP-30. The accuracy of NMR signals integration for mixtures of safflower oil and safflower biodiesel and the use of UV-Vis spectroscopy associated with a bench-top accelerated oxidation system to investigate the performance of phenolic and amine antioxidants in safflower and babassu biodiesel were explored for the first time, showing results close to the standard methods. Therefore, 1H NMR and UV-Vis spectroscopies could be applied as alternatives to the GC and Rancimat® methods to determine conversion and monitor the oxidative stability of biodiesel rapidly and practically.
将 1H NMR 和 UV-Vis 作为评估生物柴油转化和氧化稳定性的分析技术
本研究评估了 1H NMR 和紫外可见光谱作为分析技术在表征和确定生物柴油转化率以及监测生物柴油样品与抗氧化剂的氧化稳定性方面的适用性。在这项研究中,通过酯交换反应获得了红花和巴巴苏生物柴油,理化性质证实了这两种反应的成功。生物柴油转化率的一致性很好,红花生物柴油和巴巴苏生物柴油的转化率相差在 2% 到 0.4% 之间,巴巴苏生物柴油的转化率相差 1.9%。至于紫外可见光谱,该技术与 Rancimat® 方法显示出相同的趋势,在评估红花生物柴油的氧化稳定性以及抗氧化剂 BHT 和 DMP-30 的性能方面显示出高效率。首次探讨了红花油和红花生物柴油混合物核磁共振信号整合的准确性,以及使用紫外可见光谱与台式加速氧化系统相结合来研究红花和巴巴苏生物柴油中酚类和胺类抗氧化剂的性能,结果与标准方法接近。因此,1H NMR 和 UV-Vis 光谱法可作为气相色谱法和 Rancimat® 方法的替代方法,用于快速、实用地确定生物柴油的转化率并监测其氧化稳定性。
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