Abstract
A method for the determination of lead in illicit heavy drugs by electrothermal atomic absorption spectrometry using palladium as a chemical modifier was developed. A sample of drug, 0.5 g, was dissolved in 2 ml of HNO 3 35.0% (v/v), diluting to 10 ml with ultrapure water. First, a comparative study of palladium, magnesium and palladium-magnesium used as chemical modifiers was carried out, and it was found that palladium alone is adequate to stabilize lead at a charring temperature of 1000 ° C. The optimum atomization temperature was 2400 ° C. A study on the insertion of a cool-down step before the atomization step and a study on the omission of the charring step were made. Neither approach was advantageous. A limit of detection of 31.4 μg kg −1 and a characteristic mass of 24.4 pg were obtained, with analytical recoveries between 98.0 and 105.0% for a 2.5–40 μg l −1 concentration range. The within-batch precision ( n = 11) was oscillated between 6.4 and 0.2% for a drug solution spiked with 0 and 40 μg l −1, respectively. Finally, a study of some interferences, and a study of the precision and analytical recovery on the amount of sample were also carried out.
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