Micro Dry Ashing for Trace Selenium Determination in Organic Matrices

Abstract

A specific sample treatment method was established for determination of ng levels of Selenium in microquantities of organic compounds. Our task was determination of Selenium traces, in a new pharmaceutical product, as a result of a laboratory scale synthesis, in an amount of several tens of mg. GFAAS was chosen as an analysis method, due to its sensitivity and rapidity. Among the wet and dry methods for organic material digestion tried, the low temperature dry ashing using ashing aid, was the only one which gave satisfactory recoveries of Selenium. Micro dry ashing was performed, using an Ethanol solution of Magnesium Nitrate on samples spiked with Selenium Nitrate in the range of concentration of 1–6ng mg⁻¹ at a temperature of 450°C for two hours. The presence of Magnesium Nitrate and the heating suppress the atomization with approximately 15–25%. Recoveries of Selenium varies as a function of the organic matrix: for polyaromate compounds as Chrysene and Fluoranthene they lie between 90–103% and for oxygenated compounds as Dimethoxybenzoic acid or Phthalates 23–50% respectively. Another aspect of chemical interference by organic matrices and the way how to overcome it, has been clarified.