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Quantitative moisture measurements in lubricating oils by FTIR spectroscopy combined with solvent extraction approach

机译:FTIR光谱结合溶剂萃取法定量测量润滑油中的水分

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Quantitative measurements of moisture in mineral and synthetic polyol ester based lubricating oils using FTIR spectroscopy combined with solvent extraction approach are described. The samples are prepared by mixing dry dimethyl sulfoxide (DMSO) and lubricating oils, and after phase separation, the extracted bottom DMSO layers are analyzed with FTIR. The results from the solvent extraction show that the DMSO is an excellent aprotic solvent for water removal from lubricating oils. The spectroscopic data reveal that near IR region (5400-4800cm~(-1), molecular water) gives the best results for water determination in both mineral and synthetic lubricants, followed by mid-IR region (3800-3200cm~(-1), O-H stretching). However, the water content estimated from the IR region (1800-1550cm~(-1), O-H bending) has the lowest accuracy due to the interference from aminic, phenolic additives and other oxidation products present in the lubricants. The accuracy of the FTIR spectroscopy combined with solvent extraction approach is exemplified by monitoring the water content in mineral oil during oxidation process at 150°C for 30days. The quantitative determination of the moisture in the fresh and oxidized oils by the developed approach is shown to be an alternative technique to Karl Fischer titration.
机译:描述了使用FTIR光谱结合溶剂萃取方法对矿物和合成多元醇酯基润滑油中的水分进行定量测量。通过将干燥的二甲基亚砜(DMSO)和润滑油混合来制备样品,然后进行相分离,然后用FTIR分析提取的底部DMSO层。溶剂萃取的结果表明,DMSO是从润滑油中去除水的优异非质子溶剂。光谱数据表明,在矿物润滑剂和合成润滑剂中,IR区域(5400-4800cm〜(-1),分子水)附近的水测定结果最好,其次是IR中部区域(3800-3200cm〜(-1)) ,OH拉伸)。但是,由于润滑剂中存在的胺类,酚类添加剂和其他氧化产物的干扰,从IR区域(1800-1550cm〜(-1),O-H弯曲)估计的水含量精度最低。 FTIR光谱结合溶剂萃取方法的准确性可以通过在150°C的氧化过程中监测30天矿物油中的水含量来举例说明。通过开发的方法定量测定新鲜和氧化油中的水分是卡尔费休滴定法的替代技术。

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