Analytical Sciences

Determination of Refractory Elements in Used Lubricating Oil by ICPOES Employing Emulsified Sample Introduction and Calibration with Inorganic Standards

Roseli Martins SOUZA, Carmem Lúcia P. da SILVEIRA, and Ricardo Queiroz AUCÉLIO 

Departamento de Química, Pontifícia Universidade Católica do Rio de Janeiro (PUC-RJ), Rio de Janeiro, 22453-900, Brazil

The quantification of trace elements in used lubricating oil is useful for evaluating the wearing of specific components of engines. In the present work, inductively coupled plasma optical emission spectrometry (ICPOES) was used for determining five refractory elements (Ni, Mo, Cr, V and Ti) in lubricating-oil samples. The methodology was developed while aiming at the introduction of such organic samples into the ICP as emulsions. Several nebulization systems were tested with clear advantage for Meinhard K3 coupled with a cyclonic spray chamber. The carbon deposition on the injector tip as well as the plasma background was minimized through careful optimization of the Ar and O₂ gas mixture flows into the plasma. The optimization of instrumental and experimental parameters allowed quantification using calibration curves prepared with analyte inorganic standards. An internal standard (Sc) was used to correct the matrix effects and signal fluctuations. The limits of detection (3S_b/m), in the ng g^-1 range were obtained for all five elements. The methodology was validated through an analysis of standard reference materials (SRM 1084a, 1085a and 1085b). Good analyte recoveries (from 92.6 to 104.7%) were achieved. Comparison studies against established ICPOES methodologies (sample acid decomposition or sample direct dilution in an organic solvent) have shown that the proposed methodology present clear advantages in terms of simplicity of sample preparation, overall analysis time, and the use of inorganic standards for calibration instead of expensive metallorganic standards.

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