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首页> 外文期刊>Journal of the Brazilian Chemical Society >Evaluation of Digestion Procedures for Simultaneous Determination of Ca, P, Mg, K and Na in Biodiesel by Inductively Coupled Plasma Optical Emission Spectrometry
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Evaluation of Digestion Procedures for Simultaneous Determination of Ca, P, Mg, K and Na in Biodiesel by Inductively Coupled Plasma Optical Emission Spectrometry

机译：电感耦合等离子体发射光谱法同时测定生物柴油中钙，磷，镁，钾和钠的消解程序的评价

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摘要

In the present work, the efficiency of two procedures for the digestion of biodiesel was investigated for the simultaneous determination of Ca, P, Mg, K and Na by axial view ICP OES. In the open system with conventional heating, concentrated nitric and sulfuric acids were added to the samples, and the addition of hydrogen peroxide completed the digestion. In the microwave-assisted closed system, complete digestion was performed using concentrated nitric acid and hydrogen peroxide. The analytical performances were evaluated through limits of quantification, precision of the overall procedures, final acidity of the digests, and residual carbon contents. The contents of residual carbon for the biodiesel samples digested were 0.358 +/- 0.012% using the open system with conventional heating and 0.614 +/- 0.023% using the microwave-assisted closed vessel system, demonstrating the high efficiency of both proposed procedures. The optimized microwave-assisted decomposition procedure produced the fastest, safest and most accurate analytical results with recoveries of 89.0-103.0% and deviations lower than 5% in most cases. Low limits of detection were obtained (<= 0.40 mu g g(-1)), adequate for the established limits set out in Brazilian legislation for these analytes. Three biodiesel samples produced from different oil sources were analyzed. In comparison with other procedures proposed in the literature, the developed procedure using the microwave-assisted closed system is advantageous because it neither require organic standard solutions for calibrations nor use toxic organic solvents.
机译：在目前的工作中，通过轴向观察ICP OES同时研究了两种消化生物柴油的效率，以便同时测定Ca，P，Mg，K和Na。在采用常规加热的开放系统中，将浓硝酸和硫酸添加到样品中，并添加过氧化氢完成了消解过程。在微波辅助封闭系统中，使用浓硝酸和过氧化氢进行完全消化。通过定量极限，整个过程的精度，消化液的最终酸度和残留碳含量来评估分析性能。使用常规加热的开放系统，消化的生物柴油样品的残留碳含量为0.358 +/- 0.012％，而采用微波辅助的密闭容器系统则为0.614 +/- 0.023％，这表明两种方法均具有很高的效率。优化的微波辅助分解程序可产生最快，最安全和最准确的分析结果，在大多数情况下，回收率为89.0-103.0％，偏差低于5％。获得的检测限很低（<= 0.40 g g（-1）），足以满足巴西立法中对这些分析物的既定限制。分析了从不同油源生产的三种生物柴油样品。与文献中提出的其他程序相比，使用微波辅助封闭系统开发的程序具有优势，因为它既不需要有机标准溶液进行校准，也不需要使用有毒的有机溶剂。

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