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

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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%.