Determination of acid number and base number in lubricants by Fourier transform infrared spectroscopy.

This paper describes the development of practical Fourier transform infrared (FT-IR) methods for the determination of acid number (AN) and base number (BN) in lubricants through the combined use of signal transduction via stoichiometric reactions and differential spectroscopy to circumvent matrix effects. Trifluoroacetic acid and potassium phthalimide were used as stoichiometric reactants to provide infrared (IR) signals proportional to the basic and acidic constituents present in oils. Samples were initially diluted with 1-propanol, then split, with one half treated with the stoichiometric reactant and the other half with a blank reagent, their spectra collected, and a differential spectrum obtained to ratio out the invariant spectral contributions from the sample. Quantitation for AN and BN was based on measurement of the peak height of the v(C = O) or v(COO) absorptions, respectively, of the products of the corresponding stoichiometric reactions, yielding a standard error of calibration of < 0.1 mg KOH/g oil. The AN/BN FT-IR methods were validated by the analysis of a wide range of new and used oils supplied by third parties, which had been analyzed by ASTM methods. Good correlations were obtained between the chemical and FT-IR methods, indicating that the measures are on the whole comparable. From a practical perspective, these new FT-IR methods have significant advantages over ASTM titrimetric methods in terms of environmental considerations, sample size, and speed of analysis, as well as the variety of oil types that can be handled. FT-IR analysis combining stoichiometric signal transduction with differential spectroscopy may be of wider utility as an alternative to titration in the determination of acid or basic constituents in complex nonaqueous systems.