This work proposes
a flame atomic absorption spectrometry (FAAS)
method for Fe, Cu, Zn, Al, and Cr determination in biodiesel using
water in oil (w/o) microemulsion (ME) as a sample preparation method.
A less toxic solvent (n-propanol), instead of those
used in the standard method (ABNT NBR 15556), the absence of surfactant,
and calibration using inorganic reference standards were investigated.
A ternary phase diagram of biodiesel as oil, water, nitric acid, and n-propanol showed a single-phase ME region. The composition
of ME adopted for analysis was 1.7 g of biodiesel and 1.1 mL of 1.4
mol L–1 HNO3, completed with n-propanol to 10 mL volume. Linear calibration graphs with R > 0.99 were obtained using ME prepared with oleic acid
and inorganic standards. Analytes were stable for at least 3 days
both in sample and in metallic standards MEs. The limits of detection
obtained were 0.3, 0.1, 0.07, 1.7, and 1.0 mg kg–1 for Fe, Cu, Zn, Al, and Cr, respectively. These limits of detection
were lower than those obtained by the reference method of dilution
with organic solvent, due to lower fluctuation in the measurements.
Recovery test values (93–105%) indicated absence of matrix
effects. In order to assess the method accuracy, several real samples
were analyzed by the proposed method, by the standard method, and
also by acid digestion, without significant differences between results
when applying the student’s t test. Relative
standard deviations lower than 5% were obtained for standard and samples
MEs. Therefore, combination of w/o ME with the FAAS technique and
calibration with inorganic standards proved to be an accurate, simple,
fast, and practical strategy, with greater analyte stability and appropriate
sensitivity, so that the proposed method is suitable for biodiesel
routine analysis.