Detailed characterisation of sulphur and nitrogen components in a multifunctional,ashless lubricant additive by spectroscopic and chromatographic techniques

The work reported here used infrared (IR), multinuclear nuclear magnetic resonance (NMR), and chromatographic techniques to identify and characterise a commercial sulphur‐ and nitrogen‐containing ashless multifunctional additive. The proper assignment of signals in the ¹H/¹³C NMR and IR spectra of the sample has facilitated the identification of different types of sulphur‐ and nitrogen‐containing components. The methodology involves investigation by NMR and IR spectroscopies, thin‐layer chromatography (TLC) and high‐performance liquid chromatogaphy (HPLC) techniques to elucidate the types of components present. This requires the generation of NMR and IR spectral data for standard compounds of alkyl sulphides with different sulphur content and alkyl chain, and nitrogen and sulphur components such as thiadiazole, imidazoline, triazole, etc., and spectral comparison with the spectra of the unknown sample. Further, these components have been separated by silica/alumina column chromatographic and preparative TLC techniques and subsequently analysed for their exact chemical structure by spectroscopic techniques. The combined spectroscopic and chromatographic analyses have yielded the presence of four types of components: di‐t‐octyl polysulphide, di‐t‐octyl thiadiazole, a component containing amine ether functionality, and alkyl amine salts of mono/dialkyl phosphoric acid.