A modified standard addition method in X-ray fluorescence spectrometry

Abstract

A modified standard addition method for single element determination by X-ray fluorescence spectrometry has been studied. The attenuation properties of the standard added samples are kept constant by adding decreasing amounts of an attenuation modifier along with increasing amounts of a standard. In this way the standard addition curve will be a straight line in cases where the ordinary standard addition curve is non-linear, and linear regression can be used to evaluate the concentration of the analyte. Standard additions of oxides of a number of elements, with and without modifier, have been made to cellulose powder or a mixture of aluminium oxide and polyethylene as matrices in order to test the method. The method has been applied to the determination of zinc in fly-ash from a steel work and of iron in cement. The fly-ash contained about 5% of zinc and the cement samples between 2 and 5% of Fe 2O 3. The results were compared with those obtained by ICP-AES after decomposition of samples in lithium tetraborate or lithium metaborate and dissolution of the melt in 10%(v/v) nitric acid. The results agreed within 2%, relative, for fly-ash and within 3–6%, relative, for cement samples.