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Preparative isolation and characterization of zinc dialkyldithiophosphates from commercial antiwear additives
Author(s) -
Carbognani Lante
Publication year - 2003
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200301471
Subject(s) - chromatography , high performance liquid chromatography , chemistry , repeatability , elution , lubricant , zinc , fraction (chemistry) , characterization (materials science) , materials science , organic chemistry , nanotechnology
Abstract An automated HPLC separation methodology was developed for the preparative separation of ZnDTP components from commercial lubricant antiwear additives. Using silica columns that can be reactivated by elution with appropriate solvents, gram quantities of additives can be isolated. The isolated materials are useful for carrying out further mechanistic and synthetic studies. Preliminary estimations suggest that separation repeatability and fraction recoveries have acceptable levels. Qualitative characterization of isolated ZnDTP mixtures was achieved by IR, TLC‐FID, and RP‐HPLC. IR is useful for assessing the nature of ZnDTP alcoholic moieties. TLC‐FID provides a check on the preparative HPLC separation efficiency. RP‐HPLC on octadecylsil‐silica columns provides fingerprints for isolated commercial ZnDTP active concentrates. Fingerprinting on small bore HPLC columns proved advantageous compared with conventional columns.