Determination of major, minor and trace elements in cobalt-substituted lithium nickelate ceramic powders by inductively coupled plasma optical emission spectrometry |
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Authors: | Yodalgis Mosqueda Mario Pomares Eduardo L Pérez-Cappe Avelina Miranda Juan C Fariñas María T Larrea |
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Institution: | (1) Instituto de Ciencia y Tecnología de Materiales, Universidad de la Habana, 10400 La Habana, Cuba;(2) Centro de Espectrometría Atómica, Universidad Complutense, 28040 Madrid, Spain;(3) Instituto de Cerámica y Vidrio (CSIC), Campus de Cantoblanco, 28049 Madrid, Spain;(4) Centro Nacional de Investigaciones Metalúrgicas (CSIC), 28040 Madrid, Spain |
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Abstract: | An analytical method was developed for the determination of three major (Li, Ni and Co) and fourteen minor or trace elements
(Al, Ba, Ca, Cu, Cr, Fe, K, Mg, Mn, Na, Si, Sr, Ti and V) in LiNi1−x
Co
x
O2 (x = 0.2–0.8) ceramic powders by inductively coupled plasma optical emission spectrometry. Sample dissolution was achieved by
25% nitric acid digestion in a microwave oven. For each element, an analytical line free from spectral interferences was selected.
A detailed study of matrix effects over a wide interval of total excitation energy (TEE) lines (1.62–16.50 eV) was performed
at near-robust plasma conditions. A remarkable enhancement in atomic lines with TEE <4 eV was noticed, whereas a significant
reduction in atomic and ionic lines with TEE >4 eV was observed. The extrapolation to infinite dilution method was successfully
used to overcome these nonspectroscopic interferences. Detection limits (3σ) varied from 0.21 mg kg−1 for Sr to 49.7 mg kg−1 for Na. The precision of determination (obtained as the relative standard deviation) was lower than 1% for the major elements
Li, Ni and Co and between 0.69 and 10% for minor and trace elements. The accuracy of the method ranged from 91 to 101% for
major elements, and from 90 to 110%, or close to this range, for most of the impurities in both of the samples studied.
![MediaObjects/216_2006_788_Figa_HTML.gif](/content/a6j4371k133k5152/MediaObjects/216_2006_788_Figa_HTML.gif) |
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Keywords: | Cobalt-substituted lithium nickelate ceramic ICP– OES Elemental determination Matrix effect correction Extrapolation to infinite dilution method |
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