Optymalizacja warunków oznaczania wody metodą miareczkowania kulometrycznego z odparowaniem dla olejów smarowych

Abstract

The knowledge of the water content of various petroleum products, including lubricating oils, additives and various innovative products, is important from the point of view of manufacturing, purchasing or selling them, due to the impact on their quality and performance characteristics. In the case of lubricating oils, the presence of water can lead to premature corrosion and wear, the formation of deposits, which leads to reduced lubrication and premature clogging of filters, reduced action of additives or undesirable bacterial growth. The article presents the study on the selection of optimal conditions for the determination of water content by coulometric Karl-Fischer titration with evaporation in lubricating oils. The tests were carried out using a coulometer with a titration cell without a diaphragm by Metrohm, 917 Coulometer model with an automatic sample feeder equipped with a heating chamber 885 Compact Oven Sample Changer. Various types of lubricating oils were selected for testing, namely engine oils of different viscosity classes (5W/40, 10W/40, 15W/40, 5W/30), gear oil, hydraulic oil, turbine oil, base oil and hydraulic fluid. All selected samples of lubricating oils were tested in four different measuring conditions: 110°C and 20 ml/min; 150°C and 50 ml/min, 180°C and 50 ml/min and 150°C and 70 ml/min. It was found that for all the lubricating oils, the best results were obtained with a furnace temperature setting of 150°C and a carrier gas flow of 50 ml/min or 70 ml/min. The influence of various factors, such as the sample weight, the furnace temperature, the carrier gas flow velocity on the test course and the analysis speed, was determined. Increased carrier gas flow of up to 70 ml/min does not shorten the analysis time. In some cases, an increase in the oven temperature may speed up the analysis, but this is quite risky for some samples that decompose at given temperature. It is therefore safer to conduct the test at an oven temperature of 150°C. The speed of analysis is most influenced by an appropriate selection of the sample quantity under analysis. Depending on the water content in the tested sample, the appropriate sample weight should be selected. It should be small enough not to excessively extend the analysis, but also large enough that the amount of titrated water is at least twice as large as in the blank.