Reference-material-based collaborative test of flame atomic absorption spectroscopic determination of calcium and magnesium in foods and biological materials.

A flame atomic absorption spectroscopic (FAAS) method is described for the determination of calcium and magnesium in a wide variety of foods and biological substrates. Results for reference materials (n = 9) are presented that demonstrate the validity of the procedure. Samples are digested with nitric acid at 150 degrees C in a pressure decomposition vessel, diluted and adjusted to pH 2 with ammonia. Lanthanum chloride solution is added to suppress phosphate interferences and the ionization of calcium and magnesium in the AAS flame. Additional dilutions are made as appropriate, whereupon the atomic absorption of calcium and magnesium is measured in an oxidizing air-acetylene flame. The wavelength settings for calcium is 422.7 nm and for magnesium 285.2 nm. The method was tested in a collaborative trial involving a milk powder practice sample and four test samples, all of which were reference materials. Participants were requested to carry out duplicate determinations exclusively. Results were obtained from 12 laboratories. However, the results of 3 laboratories had to be rejected for various reasons. The remaining set of data was statistically evaluated according to ISO 5725; the method of analysis proved to be precise and accurate. Coefficients of variation values for calcium ranged from 1.19% to 4.44% within laboratories (CVr) and from 5.30% to 15.9% between laboratories (CVR). For magnesium, the corresponding values were CVr, 1.07% to 3.52% and CVR, 3.07% to 5.99%. The method is recommended for the determination of calcium and magnesium at the levels considered in foods and biological substrates.