Method for analyzing engine oil degradation

• US 8,087,287 B2
• Filed: 11/11/2008
• Issued: 01/03/2012
• Est. Priority Date: 11/11/2008
• Status: Expired due to Fees

• Current Assignee: GM Global Technology Operations LLC (General Motors Company)
• Original Assignee: GM Global Technology Operations LLC (General Motors Company)
• Inventors: Cummings, Jill M.
• Primary Examiner(s): LARKIN, DANIEL SEAN
• Application Number:
  US12/268,666
• Publication Number:
  US 20100116022A1
• Time in Patent Office: 1,148 Days
• Field of Search: 73/233.7, 73/233.8, 73/234.1, 73/530.5, 73/615.2, 73/615.5, 73/615.8, 436/60
• US Class Current: 73/53.05
• CPC Class Codes: G01N 33/2876 Total acid number
• CPC Class Codes: G01N 33/2888 Lubricating oil characteristics, e.g. deterioration lubricating properties G01N33/30

Abstract

The present disclosure provides a method for detecting degradation of an engine oil, by separation into a polar component and a non-polar component via admixture with a polar solvent having a polarity index greater than or equal to 5 and optionally a non-polar solvent having a polarity index of less than or equal to about 1. The polar component is analyzed for one or more degradation indicators selected from the group consisting of antioxidants, acid content, and combinations thereof. Such degradation indicators relate to a degree of engine oil degradation. The polar component may be analyzed by Gas Chromatography and Mass Spectrometry (GC/MS) for the one or more degradation indicators, which can provide a semi-quantitative level of such degradation indicator species. The non-polar component identifies combustion products that help to explain the level of degradation.

Claims

1. A method for detecting degradation of an engine oil comprising:

separating an engine oil sample into a polar component and a non-polar component; and

analyzing the polar component for one or more degradation indicators selected from the group consisting of antioxidants, acid content, and combinations thereof, wherein said degradation indicators relate to a degree of engine oil degradation.

2. The method according to claim 1, wherein said separating comprises extracting said polar component with a polar solvent having a polarity index greater than or equal to five.

3. The method according to claim 2, wherein said polar solvent comprises methanol.

4. The method according to claim 1, wherein said separating comprises extracting said non-polar component with a non-polar solvent having a polarity index of less than or equal to about one.

5. The method according to claim 4, wherein said non-polar solvent comprises heptane.

6. The method according to claim 1, wherein said separating further comprises admixing said engine oil sample with said polar solvent to form a first mixture;

agitating said first mixture; and

permitting said first mixture to settle for at least twenty-four hours.

7. The method according to claim 6, wherein said admixing further comprises mixing said engine oil sample with a non-polar solvent and said polar solvent to form said first mixture.

8. The method according to claim 1, wherein said analyzing of said polar component is conducted by gas chromatography and mass spectrometry (GC/MS).

9. The method according to claim 8, wherein a gas chromatography column used during said gas chromatography (GC) comprises 5%-phenyl-95% dimethylpolysiloxane.

10. The method according to claim 8, wherein said analyzing comprises heating said polar component to a predetermined temperature of about 200°

C. during said gas chromatography.

11. The method according to claim 10, wherein said analyzing further comprises heating said engine oil sample to a second predetermined temperature of about 300°

C. after said predetermined temperature.

12. The method according to claim 8, wherein said analyzing of said polar component further comprises Flame Ionization Detection (FID) after said gas chromatography and mass spectrometry (GC/MS).

13. The method according to claim 1, wherein said one or more degradation indicators is selected from the group consisting of 2,6-di-tertiary-butyl phenol, 2,6-di-tert-butyl-4-methylphenol, diphenylamine, phenyl-alpha-naphthylamine, 4,4′

-(1,2 ethenediyl) bis-benzenamine, butylated-octylated diphenylamine, 4,4′

-methylenebis [2,6-bis 1,1-dimethylethyl] phenol, octylated diphenylamine, bis-nonyl diphenylamine, and combinations thereof.

14. The method according to claim 1, wherein said one or more degradation indicators comprises one or more carboxylic acids.

15. A method for detecting engine oil degradation comprising:

determining a first amount of one or more degradation indicators selected from the group consisting of antioxidants, acid content, and combinations thereof in a first engine oil composition, by separating said first engine oil composition into a polar component and a non-polar component and analyzing said polar component, wherein said first amount of said one or more degradation indicators relates to a degree of degradation of said first engine oil composition;

determining a second amount of one or more degradation indicators selected from the group consisting of antioxidants, acid content, and combinations thereof in a second engine oil composition that is distinct from said first engine oil composition, by separating said second engine oil composition into a polar component and a non-polar component and analyzing said polar component, wherein said second amount of said one or more degradation indicators relates to a degree of degradation of said second engine oil composition; and

comparing said first amount of said one or more degradation indicators to said second amount of said one or more degradation indicators to determine the relative engine oil degradation of said first oil composition as compared to said second oil composition.

16. The method according to claim 15, wherein said separating said first engine oil composition comprises admixing said first engine oil composition with both a non-polar solvent comprising heptane and said polar solvent comprising methanol so as to extract said polar component with said polar solvent comprising methanol from said first engine oil composition, and said non-polar component with said non-polar solvent comprising heptane from said first engine oil composition, and said separating said second engine oil composition further comprises admixing said second engine oil composition with both said non-polar solvent comprising heptane and said polar solvent comprising methanol so as to extract said polar component from said second engine oil composition with said polar solvent and said non-polar component with said non-polar solvent from said second engine oil composition.

17. The method according to claim 16, wherein said separating further comprises admixing said first engine oil composition with said polar solvent and said non-polar solvent to form a first mixture;

agitating said first mixture; and

permitting said first mixture to settle for at least twenty-four hours and said separating of said second engine oil composition further comprises admixing said second engine oil composition with said polar solvent and said non-polar solvent to form a second mixture;

agitating said second mixture; and

permitting said second mixture to settle for at least twenty-four hours.

18. The method according to claim 15, wherein said determining comprises analyzing said first engine oil composition polar component and said second engine oil composition polar component separately by gas chromatography and mass spectrometry (GC/MS), wherein a GC column of said GC/MS comprises 5%-phenyl-95% dimethylpolysiloxane.

19. The method according to claim 15, wherein said one or more degradation indicators is selected from the group consisting of 2,6-di-tertiary-butyl phenol, 2,6-di-tert-butyl-4-methylphenol, diphenylamine, phenyl-alpha-naphthylamine, 4,4′

-(1,2 ethenediyl) bis-benzenamine, butylated-octylated diphenylamine, 4,4′

-methylenebis [2,6-bis 1,1-dimethylethyl] phenol, octylated diphenylamine, bis-nonyl diphenylamine, carboxylic acids, and combinations thereof.

20. A method for detecting degradation of an engine oil comprising:

admixing an engine oil sample with a polar solvent comprising alkanol to form a mixture;

agitating said mixture; and

permitting said mixture to separate for at least twenty-four hours to form a polar component and a non-polar component; and

analyzing said polar component by gas chromatography/mass spectrometry (GC/MS) to determine a presence of one or more degradation indicator species selected from the group consisting of antioxidants, acid content, and combinations thereof, which relate to a degree of engine oil degradation.

21. The method according to claim 20, wherein said gas chromatography (GC) employs a column comprising 5%-phenyl-95% dimethylpolysiloxane.

22. The method according to claim 20, wherein said antioxidant degradation indicator species is selected from the group consisting of 2,6-di-tertiary-butyl phenol, 2,6-di-tert-butyl-4-methylphenol, diphenylamine, phenyl-alpha-naphthylamine, 4,4′

-(1,2 ethenediyl) bis-benzenamine, butylated-octylated diphenylamine, 4,4′

-methylenebis [2,6-bis 1,1-dimethylethyl] phenol, octylated diphenylamine, bis-nonyl diphenylamine, carboxylic acids, and combinations thereof.