Fast and simplified determination of PCA and aromatic carbon content of treated distilled aromatic extract (TDAE) by NMR

Aromatic oils obtained during lubricant production (DAE) have high value as rubber extenders in tire manufacturing, but they have high carcinogenic potential due to the content of polycyclic aromatic compounds (PCAs). Legislation on PCA content requires additional treatment to reach treated oils (TDAE) with a PCA content lower than 3% according to the IP 346 method. IP 346 is a highly time-consuming and high uncertainty method, and several proposals have tried to replace it, but nowadays, there is no standard alternative. In this work, an extensive collection of samples covering a broad PCA content were obtained and characterized by physical properties, NMR, and aromatic and PCA content. Several correlations were tested to establish an optimum procedure to estimate the aromatic and the PCA content according to the requirement of high accuracy and low time and effort. The combination of several properties does not improve the accuracy of the correlation, and simpler equations were preferred. Integrated spectra appear as an acceptable characterization method as NMR percent of the total aromatic proton and polycyclic aromatic proton correlates satisfactory with the number of aromatic carbons and PCA content, respectively. The refractive index yields the best results for the correlation to PCA content. Obtained deviations compare favorably with methods previously described in the literature and with the uncertainty involved in the experimental method. They can be considered adequate methods to analyze such magnitudes routinely. Graphical abstract