Comparison between SS-ETV-ICP-OES and the tradistional nebulization ICP-OES technique for multi-element analysis of cementitions material

Abstract

SUMMARY IN ENGLISH In this study, a method development was performed for the analyses of the total concentration of major, minor and trace elements in cement and concrete materials with an inductively coupled plasma optical emission spectrometer (ICP-OES). The total concentrations should be used further in the calculation of results from different leaching experiments and subsequent geo-chemical speciation modelling in the Ph D study of Engelsen. Mainly two introduction techniques were compared, direct solid sample electrothermal vaporization (SS-ETV) with the aid of standard addition calibration and traditional nebulization of microwave-digested samples with acid-matched liquid calibration standards.

The best results were attained when analysing microwave-digested samples with traditional nebulization ICP-OES. 13 elements could be quantitatively determined in a certified cement reference material, these were (the percent recovery is given in parenthesis following the respective element or its element oxide) Al2O3 (100), Ba (85), CaO (86.0), Fe2O3 (83.8), K2O (133), MgO (98.2), Mn3O4 (101), Na2O (116), SiO2 (95), SrO (96.7), TiO2 (98.2), V (106) and Zn (93). The developed method was tested on two types of concrete samples, and the number of elements quantitatively determined for these samples were 11. These elements were the ones listed above except for SrO and Zn and V and Zn in the case of recycled concrete aggregates and laboratory concrete samples, respectively. In comparison, only one element could be quantitatively determined when solid certified cement reference material was directly analysed with the aid of an electrothermal vaporizer (i.e. ZrO2 with a percent recovery of 93%).

To overcome the different amounts of hydrofluoric acids that were needed to totally decompose cement and concrete materials, a boric acid step was included in the process of microwave digestion.