Abstract

A slurry sampling method was developed for the fast determination of Pb, Ni, Fe, and Mn in construction materials by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS). For sample introduction into the GF, stable slurries were prepared by sonicating 10 mg of ground solid sample in 10.0 mL of 1% (v/v) Triton X-100 and 1% (v/v) HNO3 solution for 1.0 min. The determination of the four elements was carried out in three measurement runs, with Ni and Fe being determined simultaneously. The HR-CS GFAAS measurements were performed using analytical lines with adequate sensitivity, considering the content of each element in the material: Pb at 283.306 nm (42%), Mn at 403.080 nm (6.7%), Ni at 232.003 nm (100%) and Fe at 232.036 nm (1.4%). The pyrolysis and atomization temperatures and the use of chemical modifiers were optimized using both aqueous standards and slurry samples. At optimal conditions, samples with concentrations of Pb from 1.5 to 80 μg g-1, Ni from 4.0 to 75 μg g-1, Mn from 2.0 to 600 μg g-1, and Fe from 0.15 to 60 mg g-1 could be determined using a unique sample suspension. To assess the validity of the method, a fly ash certified reference material (CRM) was analysed using the slurry sampling HR-CS GFAAS method; this CRM and the construction material samples were also analysed by HR-CS GFAAS after the digestion of the samples. The obtained results using both methods were statistically comparable (Student's paired t-test for two independent methods at a 95% confidence level) demonstrating the suitability of the proposed method.

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