Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

• Determination of inorganic constituents in mineral fertilizers was proposed.
• Experimental design methodology was used to optimize analytical method.
• The sample preparation procedure using diluted reagents (HNO3 and H2O2) was employed.
• The analytical method was satisfactorily to the determination of thirteen elements.
• The ICP OES technique can be used in routine analysis of mineral fertilizer samples.

An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg− 1 for Mn to 77.3 mg kg− 1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES).