Determination of macro-constituents in advanced ceramic materials by inductively coupled plasma atomic emission spectrometry

Abstract

An analytical method was developed for the determination of macro-constituents by inductively coupled plasma atomic emission spectrometry in the following six advanced ceramic materials: calcia partially stabilized zirconia (Ca-PSZ), yttria–ceria–tetragonal zirconia polycrystalline (Y-TZP/Ce), barium titanate (BaTiO₃), gadolinium-modified lead titanate (Gd-PT), lead zirconate–titanate (PZT) and lanthanum-modified lead zirconate–titanate (PLZT). The dissolution of the samples was achieved by using the following methods: decomposition with HCl in a poly(tetrafluoroethylene)(PTFE)-lined pressure vessel at 160 °C for 16 h; decomposition with HF + H₂SO₄ in a PTFE-lined pressure vessel at 170 °C for 16 h; decomposition with (NH₄)₂SO₄+ H₂SO₄ in a glass beaker; decomposition with (NH₄)₂SO₄+ H₂SO₄ in a platinum dish; fusion with Na₂CO₃+ Na₂B₄O₇ in a platinum crucible; and fusion with Li₂B₄O₇ in a graphite crucible. The precision of the determination of the macro-constituents with regard to the wavelength, integration time, dilution of the sample solution and use of an internal standard was studied. In general, the highest precision was obtained by employing the most sensible analytical line of each element, by working with elevated integration times (700–1000 ms), by diluting the sample solution 1 + 9 or 1 + 19 and by using V or Y as an internal standard. The analytical results obtained following three different methods of dissolution for each advanced ceramic material were in excellent agreement. Good precision and accuracy were attained; the relative standard deviations for the results obtained for each element for each dissolution method are <1%.