Multivariate optimization of simple procedure for determination of Fe and Mg in cassava starch employing slurry sampling and FAAS.

A slurry sampling procedure has been developed for Fe and Mg determination in cassava starch using flame atomic absorption spectrometry. The optimization step was performed using a univariate methodology for 200mg samples and a multivariate methodology, using the Box-Behnken design, for other variables, such as solvent (HNO3:HCl), final concentration (1.7molL-1) and time (26min). This procedure allowed determination of iron and magnesium with detection limits of 1.01 and 3.36mgkg-1, respectively. Precision, expressed as relative standard deviation (%RSD), was of 5.8 and 4.1% (n=10) for Fe (17.8mgkg-1) and Mg (64.5mgkg-1), respectively. Accuracy was confirmed by analysis of a standard reference material for wheat flour (NIST 1567a), which had certified concentrations of 14.1±0.5mgkg-1 for Fe and 40±2.0mgkg-1 for Mg, and the concentrations found using proposed method were 13.7±0.3mgkg-1 for Fe and 40.8±1.5mgkg-1 for Mg. Comparison with concentrations obtained using closed vessel microwave digestion was also realized. The concentrations obtained varied between 7.85 and 17.8mgkg-1 for Fe and 23.7-64.5mgkg-1, for Mg. The simplicity, easily, speed and satisfactory analytical characteristics indicate that the proposed analytical procedure is a good alternative for the determination of Fe and Mg in cassava starch samples.

Atomic spectrometric methods for the determination of metals and metalloids in automotive fuels--a review.

Gasoline, diesel, ethanol and more recently also biodiesel are the four types of fuel used for automobile, truck and other transportation vehicle. The presence of metallic and metalloid species in automotive fuels is undesirable, except in the form of additives in order to improve specific characteristics of the fuel. Metallic or metalloid elements may derive from the raw product, such as nickel and vanadium in petroleum-based fuel or phosphorus in biodiesel, or they may be introduced during production and storage, such as copper, iron, nickel and zinc in case of petroleum-based fuel and alcohol or sodium and potassium in the case of biodiesel. The most famous additive to fuel is undoubtedly lead, the use of which has been banned or drastically reduced now in many countries of the world. The problems related to the trace element content may be economic, such as fuel degradation and poisoning of automotive catalysts, and/or environmental, such as the emission of metal compounds to the atmosphere. The analytical methods that have been developed for metal and metalloid quantification in automotive fuel are reviewed in this article. The main atomic spectrometric techniques used for trace metal and metalloid determination in fuels, particularly atomic absorption spectrometry with flames, graphite furnaces and with chemical vapor generation, and inductively coupled plasma coupled with optical emission and mass spectrometry are presented, including the different sample preparation procedures proposed for these techniques.