Direct Determination of Molybdenum in Milk and Infant Food Samples Using Slurry Sampling and Graphite Furnace Atomic Absorption Spectrometry

Abstract

A fast and efficient method to determine molybdenum, Mo, in milk and other infant food by atomic absorption spectrometry with electrothermal atomization employing slurry sampling was developed. Slurries were prepared in ultrapure water with 5 to 20 min of sonication in concentrations of 10% w/v. The injection of 5.0 µL of a 0.1% (v/v) cetyl trimethyl ammonium chloride solution before the temperature program reduced the effect of build-up of carbonaceous residues within the atomizer. Europium (chemical modifier) and niobium (permanent modifier) were chosen for use from several potential modifiers. The parameters of merit were obtained in the optimized conditions Ta = 2,700 oC, Tp = 2,000 oC, tp = 20 s, and Eu 5.0 μg + permanent Nb 500.0 μg. These parameters were linear working range up to 100.0 μg/L, limit of detection (1.1 ± 0.1) μg/L, aqueous calibration, and standard addition curves with r2 > 0.9900 and relative standard deviation of 0.6% to 8.7%. The accuracy was evaluated by recovery tests and by certified material analysis; the agreement among these numbers validated the method. The powdered sample concentrations were between 39 and 1,570 µg/kg.