Properly characterizing a lubricant deposit can provide insight into the cause of a problem and allow plants to make corrective actions, resulting in tremendous savings. This webinar will present a multitude of real-world case studies where this practice of deposit characterization has been used in the field. Attendees will learn how a unique deposit that is not detectable through normal varnish testing caused a million-dollar shutdown at a nuclear facility, about the creation of tar balls in a sensitive gas turbine, how black goo was generated in a critical gas compressor, among others. (Greg Livingstone, Fluitec, 2014)

1. Lubricant Deposit Characterization
Greg Livingstone
Exec. VP Bus Development
©2013. Fluitec. All Rights Reserved.

2. Deposit Issues
Deposits cause a host of problems
Sticking valves
Plugged lubricant orifices
Plugging filters
Inefficient heat exchanger operation
Bearing Lubrication
Loss of Seals
Page 2. ©2013 Fluitec. All Rights Reserved.

3. Why do we want to Characterize
Deposits?
1. To establish a condition monitoring program
2. To discover the root cause of fluid failure
3. To take proactive actions to improve the life
and performance of your lubricants.
Page 3. ©2013 Fluitec. All Rights Reserved.

4. How do We Analyze the Deposits
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5. How do We Analyze the Deposits
Page 5. ©2013 Fluitec. All Rights Reserved.

6. Current Practices
Assume that all deposits or varnishes are
created equal.
Using visual characterization of a deposit
• assumes that since it is brown
• it must be the same as previously observed.
This assumption can be far from correct
Can lead to the wrong corrective actions.
Page 6. ©2013 Fluitec. All Rights Reserved.

7. Degradation & Deposit Formation
Oxidation
Thermal
Degradation
Contaminants
Other
Water
Additive
Drop-Out
Metal
Catalysts
MicroDieseling
Solids
Additive
Reaction Byproducts
Ultraviolet
Hot Spots
Gas
Formulation
Quality
Combustion
Incompatible
liquid
Incompatible
fluids
Air
Spark
Discharge
Page 7. ©2013 Fluitec. All Rights Reserved.

8. Analyzing the
Deposit
Page 8. ©2013 Fluitec. All Rights Reserved.

9. Characterizing
the Deposit
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10. Common to have
multiple types of
deposits in a
system.
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11. Classifying the Deposits
Deposits are classified by:
• Physical characteristics
• Source of formation
Based on this information, proactive measures
can be taken to eliminate deposit formation.
Page 11. ©2013 Fluitec. All Rights Reserved.

12. Beyond Academic – Case Studies
©2013 Fluitec. All rights reserved

13. Case Studies
1.
2.
3.
4.
Gas Turbine Tar Balls
Deposits in a Nuclear Power Plant
EHC system deposits
Dirty Gas Turbine Reservoir
Page 13. ©2013 Fluitec. All Rights Reserved.

14. 1. Gas Turbine Tar Balls
A Large Frame Gas Turbine had an oil sample
that caused concern:
Page 14. ©2013 Fluitec. All Rights Reserved.

15. Significant deposits occurred during
the outage
When the fluid temperature got below 32oC large black tar-balls were observed
floating on the lube-oil surface in the tank and clogged hydraulic filters.
Page 15. ©2013 Fluitec. All Rights Reserved.

16. An Oil Reclamation Company helped
clean up the system
Page 16. ©2013 Fluitec. All Rights Reserved.

17. The Deposits were analyzed
3391
1027
3048
1156
2854
%T
693
1459
1303
2924
766
748
Varnish Isolated Fraction 1
1385
PHENYL-A-NAPHTHYL AMINE(PANA)
4000.0
•
•
•
3600
3200
2800
2400
2000
1800
cm-1
1589
1600
1400
1200
1000
800
605.0
Decomposed amine antioxidant derived from the lubricant
formulation.
The analysis identified this material as a mixture of unreacted and
reacted PANA.
The unreacted N-H from the PANA can easily be seen in FTIR at
3391 cm-1 along with the characteristic fingerprint stretches in the
1500-700 cm-1 region.
Page 17. ©2013 Fluitec. All Rights Reserved.

18. Isolated components identified foam
inhibitor
107.6
100
90
3452
80
70
60
1648
696
50
766
%T
864
40
2968
2859
30
2925
20
732
1455
Varnish Isolated Fraction 2
Acrylate Defoamant
937
1239
1372
10
1100 1020
1735
2.7
4000.0
3600
3200
2800
2400
2000
1800
1600
1400
1200
1000
800
600
450.0
cm-1
•
•
Acrylate polymer additive typically used to control foam
This additive could not be observed in the in-service fluids
from this system – nor could it be observed in the new fluid.
Page 18. ©2013 Fluitec. All Rights Reserved.

19. Composition of the Deposits
Source:
• Formulation
derived (Amine
Antioxidant)
• Contaminant
derived (Foam
Inhibitor)
Incompatible fluid
mixed into this
system.
Page 19. ©2013 Fluitec. All Rights Reserved.

20. Gas Turbine Plant Conclusions
Deployed a quality control program to ensure
incompatible lubricants do not accidentally get
added to the system.
Page 20. ©2013 Fluitec. All Rights Reserved.

21. 2 – Deposits in a nuclear power plant
Sticking valve in a feed water pump caused an
expensive, 30-hour unplanned outage.
700-gallon reservoir using ISO
32 turbine oil.
Oil analysis results did not
reveal any problems.
•
MPC value was 16.
Deposits were gathered and
analyzed to determine their
source.
Page 21. ©2013 Fluitec. All Rights Reserved.

22. ●
Investigation
1. Removed & analyzed
deposits from valve surface
2. Concentrated and analyzed
degradation products from the oil
Ref: Livingstone, Wooton
Page 22. ©2013 Fluitec. All Rights Reserved.

23. ●
Deposit chemistry matched oil
chemistry
110
105
100
95
2924.37cm
-1
90
%T
1401.72cm
-1
1702.53cm - 1
85
838.35cm - 1
U2R16
MPC 42697
80
1116.31cm - 1
75
71
4000
3500
3000
2500
2000
1500
1000
650
cm -1
Ref: Livingstone, Wooton
Page 23. ©2013 Fluitec. All Rights Reserved.

24. ●
Unique FTIR fingerprint was identified
Carboxylic acids were present as well as primary
amides.
Doublet indicate primary amides
Ref: Livingstone, Wooton
Page 24. ©2013 Fluitec. All Rights Reserved.

25. Source:
Oxidation and
contamination
from steam
leaks
Page 25. ©2013 Fluitec. All Rights Reserved.

26. ●
Nuclear Power Plant Conclusions
Ammonia was present in the plant’s steam
chemistry.
Carboxylic Acids
Ammonia
Deposits
consisting of
Primary Amides
1. It was not feasible to remove sources of ammonia from
entering the system, but it is possible to remove acids.
2. In addition to MPC, plant is monitoring these units with
FTIR to measure acidic content and primary amide
production.
Ref: Livingstone, Wooton
Page 26. ©2013 Fluitec. All Rights Reserved.

27. 3. EHC System Deposits
Rapid filter plugging and fluid failure was
experienced at a steam turbine plant causing an
outage.
Page 27. ©2013 Fluitec. All Rights Reserved.

28. Deposits were separated and analyzed
It is common for some
EHC systems to
experience microdieseling.
This creates dark oil and
black deposits.
Strong evidence of
thermal degradation.
Page 28. ©2013 Fluitec. All Rights Reserved.

29. Fluid & Deposits were analyzed
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30. What type of thermal degradation?
ESD
Type of Deposit
Micro-Dieseling
High
Temperature
Thermoplastic
<1.0 micron soot- >1.0 micron
like particles
black particles
Black deposits indicated EHC
deposits caused by microdieseling or high temp
degradation.
Page 30. ©2013 Fluitec. All Rights Reserved.

31. Thermal Degradation
Paper Chromatography
was done to assist in
identifying particle size.
Very small particles will
go through the filter
unless varnish is present
to prevent it.
Analysis indicated it was
not from micro-dieseling.
Page 31. ©2013 Fluitec. All Rights Reserved.

32. Thermal Degradation
Microscopic
evaluation revealed
particles >5microns in size.
Page 32. ©2013 Fluitec. All Rights Reserved.

33. EHC Deposit Conclusions
Instead of fixing the assumed micro-dieseling
problem, the plant focused on potential sources of
high heat.
Malfunctioning pump was found to produce
temperatures of 500oF.
Repaired the pump, solving rapid fluid
degradation.
Page 33. ©2013 Fluitec. All Rights Reserved.

34. 4. Dirty Gas Turbine Reservoir
Very dark and wide bathtub ring, reservoir deposits and varnish through the inside of
a 7FA gas turbine.
Page 34. ©2013 Fluitec. All Rights Reserved.

35. ●
Impossible to Wipe off!
@#$&!!!
Ref: Livingstone,
Page 35. ©2013 Fluitec. All Rights Reserved.

36. ●
Deposits derived from Polyacrylate
Foam Inhibitor
99.6
90
80
70
60
%T
50
40
30
20
10
2.8
4000.0
3600
3200
2800
2400
2000
1800
1600
1400
1200
1000
800
600
450.0
cm-1
System Deposit
POLYACRYLATE DEFOMANT
Ref: Livingstone, Wooton
Page 36. ©2013 Fluitec. All Rights Reserved.

37. Conclusions
1. There are many possible modes of fluid
degradation.
2. Your condition monitoring program should be
based on the failure mode of the fluid.
3. Understanding the mode of failure allows you
to address the root cause.
4. Most importantly, don’t make assumptions!
Let the data drive the decisions.
Page 37. ©2013 Fluitec. All Rights Reserved.

38. Acknowledgements
1. Dr. Dave Wooton was involved in these root
cause analysis and has co-authored
multiple papers with me on this subject.
2. TestOil provided laboratory support to these
projects and has developed leading deposit
characterization services.
Page 38. ©2013 Fluitec. All Rights Reserved.