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Contact:

John Edwards

(203) 744-5905

Lubricant Oil Base Stock Analysis by 1H and 13C NMR

Liquid-state NMR analysis of lubricant oil base stocks yield detailed information on aromaticity, paraffinicity and naphthenicity that is not available from any other form of analysis. Detailed paraffinic branching information is readily extracted from the 13C NMR paraffin region and variation in aromaticity type is readily observed by a combination of 1H and 13C NMR. 1H-13C DEPT experiments allow ready determination of CH3, CH2, CH and quaternary carbon contents.

An example of a 1H and 13C comparison of two contrasting oils - one that passed appropriate testing and one that failed.

Here is the background of the study which also involved solid-state 2H NMR of the two samples during the MRV cooloing cycle. The 2H studies allowed differences in wax crystal structure to be observed as the wax in the oils crystallized.

During the course of lubricant property testing in the formulation of both diesel and gasoline lubricants certain base oil stocks have become associated with poor low temperature pumpability due to the formation of wax crystallization gels. Specific tests have been developed to identify these poor low temperature properties (mini-rotary viscometer (MRV)) which manifest themselves as large increases in viscosity and shear stress (the motivating force per unit area for fluid flow). The MRV test will be described later.
Two contrasting oils have been obtained:-
Oil A : readily passes the MRV test with an acceptable viscosity increase
(< 30,000 cP), and no measurable shear stress.
Oil B : fails the MRV test due to large viscosity increase (>400,000 cP) and
a large shear stress increase (300-500 Pa).
The reasons for the differences in low temperature crystallization behavior are not readily understandable from the basic physical and chemical tests which are performed on the base oils.  Thus, a study has been undertaken to attempt to identify differences between the oils that might explain this behavior.

 

Differences in the paraffinic distribution are readily observed as are differences in aromatic character.

 

For more information on this topic please contact:

John Edwards

Manager, Process and Analytical NMR Services

Process NMR Associates LLC,

87A Sand Pit Rd

Danbury, CT 06810, USA

Tel: (203) 744-5905