Automatic determination of insolubles in lubricating oils by flow injection analysis employing an LED-photometer detector.

A flow injection system is presented for the determination of the insolubles content in used lubricating oil samples. The system is based on the injection of an aliquot of the sample in a stream of organic solvent where it is dispersed, and measurement of the scattered radiation (measured as apparent absorbance) in the visible range (lambda=640nm). An LED-based photometer was used for this purpose. The whole system including sample injection and data acquisition was controlled by a personal computer. Calibration curves exhibited good linearity (h=0.415+/-0.016C+0.00+/-0.03, r(2)=0.9995, confidence level of 95%) in the range up to 2.68% (insolubles in pentane). Detection and quantification limits were respectively 0.07% and 0.16% (w/w). The method was validated by analysis of 25 real samples by the proposed method and the FTIR method finding high correlation. Waste generation and reactive consumption is much less than in the official method (ASTM D-893). The proposed method employs 25mL of kerosene per sample while the official method employs 200mL of pentane.

Determination of Zinc-Based Additives in Lubricating Oils by Flow-Injection Analysis with Flame-AAS Detection Exploiting Injection with a Computer-Controlled Syringe.

A flow-injection system is proposed for the determination of metal-based additives in lubricating oils. The system, operating under computer control uses a motorised syringe for measuring and injecting the oil sample (200 muL) in a kerosene stream, where it is dispersed by means of a packed mixing reactor and carried to an atomic absorption spectrometer which is used as detector. Zinc was used as model analyte. Two different systems were evaluated, one for low concentrations (range 0-10 ppm) and the second capable of providing higher dilution rates for high concentrations (range 0.02%-0.2% w/w). The sampling frequency was about 30 samples/h. Calibration curves fitted a second-degree regression model (r(2) = 0.996). Commercial samples with high and low zinc levels were analysed by the proposed method and the results were compared with those obtained with the standard ASTM method. The t test for mean values showed no significant differences at the 95% confidence level. Precision (RSD%) was better than 5% (2% typical) for the high concentrations system. The carryover between successive injections was found to be negligible.