Two independent digestion techniques (microwave acid digestion with HF and HCl, HNO3 and Na2O2 sintering, respectively) were applied to determine the total Sb concentration in a real soil sample and in reference materials: Icelandic Basalt (BIR-1), Cody Shale (SCo-1) and (Soil-7). ICP-MS was used to determine total antimony concentrations in the digested and the extracted solutions using external calibration and isotope dilution technique. The recoveries of Sb using HF in the acids digestion mixture in closed-vessels microwave digestion system were excellent and the concentrations are in very good agreement with certified or reported concentrations of reference materials. Using closed-vessels combined with microwave heating systems probably prevents the loss of volatile Sb compounds. The use of hydrogen fluoride with other strong acid can help dissociating insoluble antimony silicates. Different extraction reagents were tested for their ability to extract antimony using an ultrasonic bath namely: EDTA disodium salt, potassium hydroxide, citric acid monohydrate, pyridine-2,6-dicarboxylic acid, ammonium acetate, ammonium oxalate, ammonium thiocyanate, ammonium persulphate and di-ammonium hydrogen citrate. A 500 mmol L-1 solution of citric acid pH 1.08 proved to be the most efficient extractant. Optimization of the extraction conditions were investigated by studying the effect of pH, concentration, temperature, time of extraction, the ratio of sample mass to the volume of extractant and the number of consecutive extractions. As a result three consecutive extractions for a total time of 45 min at 80 ˚C was the most efficient condition for Sb extraction. Using these extraction conditions 61%, 3.7% RSD and 42%, 2.2% RSD (n=6) of the total antimony in the real soil and Soil-7 samples, respectively could be extracted.
In-situ trace element characterization of three gold reference materials using EPMA and LA-ICP-MS