Determination of metal impurities in advanced lead zirconate titanate ceramics by axial view mode inductively coupled plasma optical emission spectrometry

• Published in: Talanta (Oxford) 2012-05, Vol.94, p.50-57
• Main Authors: Villanueva Tagle, M.E., Larrea Marín, M.T., Martin Gavilán, O., Durruthy Rodríguez, M.D., Calderón Piñar, F., Pomares Alfonso, M.S.
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Argon; Axial view mode ICP-OES; Ceramics; Ceramics - chemistry; Chemistry; Chromium; Emission; Exact sciences and technology; Hydrofluoric Acid - chemistry; Hydrogen Peroxide - chemistry; Inductively coupled plasma; Lead - chemistry; Lead zirconate titanates; Limit of Detection; Line intensity; Matrix effect; Metals - analysis; Microwaves; Nitric Acid - chemistry; PZT ceramic impurities; Signal-to-background ratio; Spectrometric and optical methods; Spectrometry; Spectrophotometry, Atomic; Spectroscopy; Titanium - chemistry; Zirconium - chemistry
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2012.02.045

► ICP-OES method has been developed for analysis of PZT ceramics. ► Influence of operating parameters on SBR, net signal intensity and matrix effect was studied. ► Some lines with an anomalous behaviour were observed. ► The precision of analysis ranged from 3 to 13%. ► The accuracy was from 90 to 110%. An inductively coupled plasma optical emission spectrometry quantification method for the determination of Al, Ca, Cr Cu, Fe, Mn, Mg, Ni, Zn, Ba, K, In and Co in lead zirconate-titanate (PZT) ceramics, modified with strontium and chromium, was developed. Total digestion of ceramics was achieved with a HNO3, H2O2 and HF (ac) mixture by using a microwave furnace. The sensitivity of the net signal intensity respect to radiofrequency power (P) and nebulizer argon flow (FN) variations was strongly dependent of the total excitation energy of line (TEE). For lines with TEE near metastable atoms and ions of argon, an increment of the sensitivities to P and FN variation was observed. At robust plasma conditions the matrix effect was reduced for all matrices and analytes considered. The precision of analysis ranged from 3 to 13%, whereas the analytes recoveries in the spiked samples varied, mostly, from 90 to 110%. The detection limits of studied elements were from 0.004 to 10mgkg−1.