Analysis of Yttria-Stabilized Zirconia by Inductively Coupled Plasma Atomic Emission Spectrometry

Аннотация

A method for determination of aluminum, hafnium, iron, yttrium, calcium, magnesium, and titanium by inductively coupled plasma atomic emission spectrometry (ICP-AES) is described. Conditions for the decomposition of two modifications of the analyzed material—unburnt and subjected to stabilizing firing—have been studied. It has been found that the unburnt zirconia dissolves in sulfuric acid, and the burnt sample can be converted to solution only by fusing with potassium pyrosulfate or potassium bifluoride. However, the application of these reagents leads to high values of the control experiment correction for trace impurities (at the level of tenths and hundredths of a percent). In this connection, we have studied the possibility of acid dissolution of the burnt sample under microwave decomposition, varying the qualitative and quantitative composition of the acid mixture, reaction temperature, and time to reach and maintain the required temperature. It has been found that the decomposition in the mixture of hydrofluoric and sulfuric acids (2 : 1) in the microwave system with stepwise heating of the reaction mixture ensures quantitative dissolution of the burnt sample and sufficiently low values of the control experiment correction for trace impurities. The analytical lines have been chosen taking into account their relative intensity, possible spectral overlaps, and the matrix effect in the analysis of model solutions containing 1.3 mg/cm³ Zr, 0.2 mg/cm³ Y, and from 0.2 to 20 mg/cm³ impurities. As a result, the following analytical lines have been chosen: Al II 167.079 nm and Al I 308.215 nm, Ca II 184.006 nm and 393.366 nm, Fe II 238.204 nm, Mg II 279.553 nm, Ti II 334.941 nm, Y II 371.030 nm, and Hf II 232.247 nm. The developed method for the analysis of yttria-stabilized zirconia by ICP-AES allows simultaneously determining aluminum, iron, magnesium, and titanium in the range of 0.01–1.0%; calcium, 0.02–1.0%; hafnium, 0.1–5.0%; and yttrium, 2.0–15% with a relative standard deviation of 6–30 rel % (for Al, Fe, Mg, Ti, and Ca), 2–7 rel % (Hg), and 2–4 rel % (Y). The correctness of the method is confirmed by the standard addition technique.