Flame AAS/flame AES for trace determination in fresh and used lubricating oils with sample introduction by hydraulic high-pressure nebulization.

In hydraulic high-pressure nebulization (HHPN) an aerosol is produced by means of an HPLC-pump and a special nebulization nozzle, applying a pressure of about 200 bar. This spray technique has been employed for sample introduction of mineral oil samples in flame atomic absorption/flame emission spectrometry. The determination of the trace elements Al, Cr, Cu, Fe, K, Na, Ni, Pb, Si and V has been investigated. Viscosity hardly acts upon the sensitivity of the determination, thereby avoiding a time consuming dilution of oil samples. By means of two interconnecting sampling valves a calibration method based on the standard addition technique can be performed which is both simple and easy to carry out. In samples of used oils, results for Cu and Pb equalled those of XRF-analysis. Regarding Fe traces, data obtained from AAS and XRF measurement correlate. In comparison with sample uptake by pneumatic nebulization, which is restricted to diluted oil samples, detection limits decrease by a factor of 2 to 4, indicating the dilution required in pneumatic nebulization.