A novel method for the sequential determination of sodium, potassium, calcium, and magnesium and free and total glycerol in biodiesel by capillary zone electrophoresis is proposed herein. The inorganic cations were separated along an effective length of 43.5 cm. The samples to quantify the free and total glycerol were injected into the opposite capillary end, close to the detection window, with an effective length of 8.5 cm. It was possible to achieve the separation of six analytes within 3 min. The quantification limits for the cations and glycerol ranged from 0.071 to 0.5 mg kg-1 to and 0.0017% to 0.017% w/w, respectively. Despite the complexity of the injection steps, the values for the instrumental, intraday and interday precision were better than 2.13, 4.49 and 5.68% (RSD), respectively, for the cations and the free and total glycerol. The method has good accuracy and specificity, which was statistically confirmed through an interlaboratory assay, where the method was compared with official methods.
Keywords: Capillary zone electrophoresis; Free glycerol; Inorganic cations; Sequential determination; Total glycerol.
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