研究目的
To explore the impact of emulsion quality on FT-IR spectroscopy calibration standards for measuring water contamination in engine oil, aiming to strengthen ASTM International guidelines for sample preparation and establish ideal techniques for reliability and reproducibility.
研究成果
Direct probe sonication is the fastest and most reliable method for creating stable emulsions for FT-IR calibration, with high reproducibility and lower variability. Other methods like pan-shaker and bath sonication with rotary mixing are viable but slower or less efficient. Emulsion stability is crucial for accurate water contamination analysis, and method choice depends on available equipment and time constraints.
研究不足
The study is limited to specific emulsification techniques and equipment; results may vary with different oils or conditions. Bath sonication showed non-uniform energy distribution, and micelle size analysis was inconclusive due to sample opacity. Generalizability to other immiscible liquids or industrial settings may require further validation.
1：Experimental Design and Method Selection:
The study compared different emulsification techniques (rotary mixing, bath sonication only, bath sonication followed by rotary mixing, pan-shaker, direct probe sonication) to assess their effects on emulsion stability and FT-IR analysis reliability. Theoretical models like Stokes' law and ANOVA were used for analysis.
2：Sample Selection and Data Sources:
Samples were prepared using fresh diesel engine oil (Shell Rotella T, SAE 15W-40) and distilled water at concentrations of 0%, 0.1%, 0.2%, 0.5%, 1%, 2%, 5%, and 10% v/v. Concentrations 0%, 0.5%, and 1% were primarily used for comparisons.
3：1%, 2%, 5%, 1%, 2%, 5%, and 10% v/v. Concentrations 0%, 5%, and 1% were primarily used for comparisons.
List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included ultrasonic processors, bath sonicators, rotary mixers, pan-shakers, FT-IR spectrometers, KBr windows, vials, pipettes, and water baths. Materials included engine oil, distilled water, acetone, methylene chloride, and parafilm.
4：Experimental Procedures and Operational Workflow:
Each sample was emulsified using specified methods (e.g., direct probe sonication for 1 min with cycling to prevent heating), stored in vials, and analyzed via FT-IR spectroscopy. Spectra were recorded, baselines adjusted, and data preprocessed. Multiple replications were performed for statistical analysis.
5：Data Analysis Methods:
Data were analyzed using ANOVA to detect significant differences, and limit of detection (LOD) and limit of quantitation (LOQ) were calculated from linear regression fits. Peak amplitudes and integrated areas of O-H stretching bands (3150-3500 cm?1) were used for quantification.
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