Determination of Na, K, Mg and Ca in Biodiesel by LS F AAS and HR-CS F AAS: Studies that Supported the Proposal of the ABNT NBR 15556 Norm

Recently, ABNT (Brazilian Association of Technical Standards) has presented a set of norms related to the determination of Na, K, Mg and Ca in biodiesel, recommending procedures similar to those of the European and American norms. However, it has also introduced an alternative norm (ABNT NBR 15556) wherein these 4 elements can be determined by flame atomic absorption spectrometry (F AAS). This work presents the studies that have supported this proposal and compares the performance of linear source equipment with a continuous source one in the application of the norm. Among the optimized factors, the low aspiration rate and the use of mineral oil solution in xylene to adjust the viscosity between samples and calibration solutions are highlighted. Precision tests (repeatability and intermediary precision) have shown adequate values, confirming the robustness of the method. Limits of detection were suitably below the legislation limits. The accuracy was confirmed by recovery tests as well as by the participation in interlaboratory proficiency tests promoted by the National Agency on Oil, Natural Gas and Biofuels (ANP, Brazil). The determination of these 4 elements by F AAS brings evident economic advantages to the producer, once F AAS is less expensive to purchase and maintenance.