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An in-depth experimental study of the matrix effect of antifreeze (ethylene glycol) and water contamination of engine oil through FT-IR spectroscopy. With a comparison of the percent by volume concentration of contaminated fresh 15W-40 engine oil, there appeared to be a noticeable reduction in the O–H stretching signal in the infrared spectrum when ethylene glycol based antifreeze was included as a contaminant. The contaminants of distilled water, a 50/50 mixture of water and commercial ethylene glycol antifreeze, and straight ethylene glycol antifreeze were compared and a signal reduction in the O–H stretch was clearly evident when glycol was present. Doubling the volume of the 50/50 mixture as compared to water alone still resulted in a weaker O–H stretching signal. The possibility that this signal reduction was due to the larger ethylene glycol molecule having fewer O–H bonds in a given sample size was eliminated by comparing samples with the same number of O–H bonds per unit volume. The strong hydrogen bonding between that of water and glycol appeared to reduce the O–H stretching signal, even after comparing the different sample types at concentrations with the same number of O–H bonds per unit volume. Tukey’s highly significant difference was used to show that samples of the 50/50 mixture and straight glycol were not reliably distinguishable from one another when comparing the same number of O–H bonds per unit volume but readily distinguishable from that of water as the lone contaminant.

Samples of gasoline engine oil (SAE 5W20) that had been exposed to various oxidation times were inspected with a UV-Visible (UV-Vis) spectrophotometer to select the best wavelengths and wavelength ranges for distinguishing oxidation times. Engine oil samples were subjected to different thermal oxidation periods of 0, 24, 48, 72, 96, 120, and 144 hours, resulting in a range of total base number (TBN) levels. Each wavelength (190.5 – 849.5 nm) and selected wavelength ranges were evaluated to determine the wavelength or wavelength ranges that could best distinguish among all oxidation times. The best wavelengths and wavelength ranges were analyzed with linear regression to determine the best wavelength or range to predict oxidation time.

Fourier Transform-Infrared (FT-IR) spectroscopy was used to analyze gasoline engine oil (SAE 5W20) samples that were exposed to seven different oxidation times (0 h, 24 h, 48 h, 72 h, 96 h, 120 h, and 144 h) to determine the best wavenumbers and wavenumber ranges for the discrimination of the oxidation times. The thermal oxidation process generated oil samples with varying total base number (TBN) levels. Each wavenumber (400–3900 cm−1) and wavenumber ranges identified from the literature and this study were statistically analyzed to determine which wavenumbers and wavenumber ranges could discriminate among all oxidation times. Linear regression was used with the best wavenumbers and wavenumber ranges to predict oxidation time.

For the most reliable and reproducible results for calibration or general testing purposes of two immiscible liquids, such as water in engine oil, good emulsification is vital. This study explores the impact of emulsion quality on the Fourier transform infrared (FT-IR) spectroscopy calibration standards for measuring water contamination in used or in-service engine oil, in an attempt to strengthen the specific guidelines of ASTM International standards for sample preparation. By using different emulsification techniques and readily available laboratory equipment, this work is an attempt to establish the ideal sample preparation technique for reliability, repeatability, and reproducibility for FT-IR analysis while still considering the ease and efficiency of the technique. This study demonstrates that a stable emulsion within a sample, which depends heavily upon the method, provides a reliably consistent homogenous sample for quantification purposes with FT-IR analysis. Analysis of variance (ANOVA) modeling and limit of detection calculations demonstrate the stability of the emulsion. The results reveal that setting a mixing time for a calibration standard depends on the emulsification process. Inserting a probe directly into a sample (direct sonication) allows for a rapid, stable emulsion with high reproducibility. Indirect sonication produces relatively non-miscible liquids of different densities. The pan-shaker produces a reasonably stable emulsion, but without the long-term stability or quick production time of direct sonication. Reaction time plays a critical role in the rotary mixing method, which leads to a slow development of emulsification.

The authors wish to correct the affiliation of co-author Ali Mazin Abdul-Munaim in their previous paper [...]

Using Fourier transform infrared (FT-IR) spectroscopy we investigated the water content of SAE 15W–40 diesel engine lubricating oil at various levels of contamination to establish instrument calibration standards for measuring water contamination in used or in-service engine oil by the standards of ASTM International. Since some known additives in consumer grade engine oil possess slightly hydrophilic properties, this experiment avoided changing the sample matrix with supplemental additives, such as adding surfactants, to achieve homogeneity of the original sample. The impact of sampling time after contamination on the spectral absorption signature was examined in an attempt to improve the accuracy of water contamination quantification and determine if water-soluble potassium bromide (KBr) windows were suitable for analyzing water in oil emulsions. Analysis of variance (ANOVA) modeling and limit of detection calculations were used to predict the ability to discriminate contamination levels over time. Our results revealed that the amount of water concentration in engine oil could be misinterpreted depending on the timing of the FT-IR measurement of the calibration standard after initial water contamination. Also, KBr windows are not sufficiently etched due to the limited window interaction with water molecules within micelles of emulsions to alter FT-IR spectral signatures.