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The use of normalized procedures designed for soil and sediment samples (like US-EPA 3051) to chemically prepare some kind of organic samples is a common practice in some laboratories. However, the performance of this method for other matrices has to be demonstrated. Three microwave-assisted digestion procedures with 0.5 g of sample and simplified reagents (10 mL HNO3 alone and mixtures of HNO3/HCl- and HNO3/H2O2 procedures A, B, and C, resp.) were compared for quantitative determination of 25 elements (Be, B, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Sr, Mo, Ag, Cd, Sb, Cs, Ba, Tl, Pb, Th and U) in three biological reference materials provided by NIST (mussel tissue (MT), tomato leaves (TL), and milk powder (MP)) by ICP-MS. From scaling masses (from 0.1 up to 0.9 g at 0.1 g interval) in procedure A, a linear relationship among instrumental signal and mass of digested sample could be constructed at 99% CL for most of the target analytes. The slope of this linear fit provided the estimation of sample concentration, while the ordinate in origin allowed the identification of matrix interferences which were absent in the reagent blank.

isrn analytical chemistry

Determination of 25 Trace Element Concentrations in Biological Reference Materials by ICP-MS following Different Microwave-Assisted Acid Digestion Methods Based on Scaling Masses of Digested Samples