Determination of Te, Bi, Ni, Sb and Au by X-ray fluorescence spectrometry following electroenrichment on a copper cathode

The electrodepositons of Te, Bi, Ni, Sb and An from aqueous solution of pH =1 on the cathode surface have been studied for X-ray fluorescence analysis (XRF). A special holder for a copper electrode has been constructed to perform the electrodeposition process on only one side of the electrode. After electrolysis, the copper electrode can be easily removed from the holder; after rinsing it with water and drying it can be analyzed by XRF. The proposed method of sample preparation and preconcentration of Te, Bi, Ni, Sb, Au provides suitable samples which are devoid of the negative and undesirable effects of XRF analysis, such as particle size and matrix effects. The influence of time on the deposition yield has been examined. The method of preconcentration is efficient. The inhomogeneity of the prepared specimens has been studied using internal standard method. The calibration is based on using synthetic standards, certified reference materials and standard addition method. The best results are achieved by the standard addition method. The agreement between results obtained with XRF analysis and certified values is satisfactory and indicates the usefulness of the proposed method for determination of Te, Bi, Ni, Sb and Au in anode slime. (c) 2007 Elsevier B.V. All rights reserved.