Measurement of water by oven evaporation using a novel oven design. 2. Water in motor oils and motor oil additives

Margolis, Sam; Vaishnav, Kevin; Sieber, John
November 2004
Analytical & Bioanalytical Chemistry;Nov2004, Vol. 380 Issue 5/6, p843
Academic Journal
The measurement of water in lubricating oils is important because water accelerates the corrosion of metal parts and bearings in motors. Some of the additives added to lubricating oils to improve their performance react with the Karl Fischer reagent (KFR) causing a positive bias in the water measurement. A new oven evaporation technique for measuring water in oils has been developed that is automated, requires less sample handling, is easily calibrated, and is capable of measuring relatively small mass fractions of water (=50 mg/kg sample). A series of motor oils was analyzed with the standard KFR, a reagent that detects interfering substances that reduce iodine, and the aldehyde-ketone reagent that does not detect substances that react with methanol and form water. The oil samples were heated to 107°C and then reheated to 160°C. At both temperatures, material was measured by both KFRs, but only zinc dithiophosphate released sulfur compounds that would react with the reagent that detects interfering substances. Mass fractions of between 20 and 70% of the volatile material released at either temperature were measured with the standard KFR but not with the aldehyde-ketone reagent. These results demonstrate that there are a number of sources of positive bias in the measurement of water in motor oils and that the standard KFR cannot be used to measure water in motor oils and motor oil additives. These results also indicate that some of the material reacts with methanol to form water. Finally, these results suggest that some of the material that is volatile at 160°C and not at 107°C may be water that is physically occluded or may be substances that react with diethyleneglycol monomethylether to produce water.


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