Systematic Bias in the Measurement of Water in Oils by Tubular Oven Evaporation and Azeotropic Distillation

Water in oil has been measured by tubular oven evaporation and by azeotropic distillation into a coulometric moisture analyzer. The results of these measurements were compared to the results obtained by volumetric titration of water in oil. The volumetric measurements were consistently higher than the measurements made by tubular oven evaporation or azeotropic distillation. A mass balance study was performed by volumetric Karl Fischer titration of the water in the oil that remained in the tubular oven and in the distillation apparatus. This study indicated that measurable amounts of water were not removed after exhaustive evaporation or distillation. The sum of the water removed by distillation from toluene and that remaining in the distillation chamber was equal to the amount of water measured in the oil by the volumetric method. The data are consistent with the existence of an oil-water azeotrope that does not release water upon evaporation at 160 °C or upon dissolution in toluene and distillation of the water-toluene azeotrope. These results were obtained for oils varying in viscosity from 8 to 850 m2/s, and the amount of water remaining associated with the oil appears to be dependent upon the composition of the oil and the method of analysis.