Validation of the cumulative or replicate NAA method for the determination of trace elements in biological materials

Abstract

To make the best use of time and facilities, a neutron activation system, fully automatic, including spectrum and data processing, to be used with short-lived nuclides, has been recently developed at the Portuguese Research Reactor (in Portuguese "Reactor Portugês de Investigação," RPI). Using this system, the cumulative neutron activation analysis method is now being implemented. This article summarizes the experimental procedures used to validate the cumulative NAA method for the determination of selenium in biological samples, emphasizing the determination of the essential characteristics of precision, accuracy, and limits of detection and of quantification of the method. The article also examines how detection limits and precision are improved when the samples are analyzed by this method compared to the cyclic activation measurements in use at RPI for the determination of selenium. The improvement is demonstrated for the measurement of selenium in several reference materials when the result obtained by adding up seven spectra of separate aliquots of the same sample is compared to the result from a cumulative spectrum of seven (whenever possible) consecutive cycles of a single sample.