Preparation and characterization of phosphate rock as quality control material

A quality control material for inorganic constituents present in a phosphate-bearing rock used to manufacture phosphate fertilizers was produced and characterized according to the ISO Guide 80. The evaluation of the estimated minimum mass, homogeneity, and stability of the material was performed using microwave-assisted digestion and inductively coupled plasma optical emission spectrometry (ICP-OES) as an in-house validated technique for determination of Al, As, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, V, and Zn. Phosphorus mass fraction determination was done by laser-induced breakdown spectroscopy. The accuracy of the measurement results was confirmed by analyzing the certified phosphate rock and fertilizer certified reference materials according to NIST SRM 694 and SRM 695. One-way analysis of variance (ANOVA) was applied to the measurement data, and the homogeneity and stability of the material presented averages within the 95 % confidence interval. The results from the preparation and with collaborative trial allowed the calculation and estimation of the consensus value and its expanded measurement uncertainties, obtained by combining the uncertainty contributions from characterization ( u char ), between-bottle homogeneity ( u bb ), short-term stability ( u sts ), and long-term stability ( u lts ) for each evaluated analyte mass fraction.