The NMR technique was used to characterize some base oils of different nature (mineral, saturated polyolefins, hydrocracked and from waxes hydroisomerization) at the molecular level. Base oils are used in the formulation of lubricants with the addition of suitable additives which improve the final products performance. The studied base oils are used particularly in the formulation of engine oils. In this paper we have compared two "NMR editing" techniques which allow one to quantify the CH" (n = 0-3) fractions of an "average" base oil molecule: 1) the gated spin echo (GASPE) and 2) the distortionless enhancement by polarization transfer (DEPT). We found that the quantitative data obtained from GASPE have a better accuracy than those from DEPT and so we chose GASPE to study the molecular characteristics of the aliphatic moieties of the base oils. On the basis of the GASPE data and of the average molecular mass obtained via VPO (Vapor Pressure Osmometry), the average number of branches and aliphatic rings were calculated. Moreover, on the basis of GASPE the distribution of side chain lengths and the positions of the methyl groups along the straight chain (methyls are the only groups for which the positions are directly obtained from NMR spectra) were obtained. A confirmation of the reliability of the NMR approach was achieved by comparing the branching degree, found with the NMR approach, of some base oils with their heats of fusion measured with the Differential Scanning Calorimetry (DSC). The heats of fusion are expected to be directly related to the length of straight CH2 sequence and therefore to be lower for more branched molecules. We found that for base oils with similar aliphatic moieties, the heats of fusion are lower for more branched base oil molecules with a nearly linear correlation. The exception to this rule is represented by the two olefinic oils. Besides, we found that the fraction of the methyls on aliphatic chains longer than three carbons, determined with GASPE, correlates very well with the pour points values, with the only exception of the mineral oil.
A new rigid liquid crystalline polymer that demonstrates good mechanical and thermomechanical properties and acceptable processing temperature has been recently synthesized and characterized. The melting temperature and some thermomechanical properties do not seem, however, suitable for use in some applications at high temperature or in the presence of aggressive fluids. The use of appropriate inorganic fillers can overcome these shortcomings. In this work the new LCP, polymerized in a bench-scale apparatus, and the same sample filled with carbon fibers are characterized. The properties of the carbon fiber filled LCP are compared with those of another filled wholly aromatic commercial LCP, a carbon filled semirigid LCP, and the same semirigid LCP reinforced with glass fibers. In general, the mechanical properties of the filled LCP sample increase remarkably when the filler concentration is about 20%; however, with further increases in filler content, a decrease is observed. The thermal and chemical resistance of this new rigid LCP seems slightly influenced by the addition of fibers, while the thermal resistance of the other two LCP samples is remarkably improved.
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