Tests for the Analysis of

Used Lubricating Grease

David Turner, CLGS, CLS, OMA
Lubricants Technical Advisor
Shell Global Solutions (US) Inc.
Houston, Texas

Copyright 2011 Shell Global Solutions

 Typical Grease Applications

• Bearings

• Gears

• Sliding Contacts

• Couplings
Copyright 2011 Shell Global Solutions
 Grease is Used in…

Copyright 2011 Shell Global Solutions

 Grease is Used in…

Copyright 2011 Shell Global Solutions

 Grease is Used in…

Copyright 2011 Shell Global Solutions

 Grease is Used in…

Copyright 2011 Shell Global Solutions

 Grease is Used in…

Copyright 2011 Shell Global Solutions

 Grease is Used in…

Anything With Moving Parts!

Copyright 2011 Shell Global Solutions

 Lubricating Grease

• The amount of grease in most applications

is small, sometimes one gram or less.

• Obtaining a representative sample of used

grease for analysis can be challenging.

Copyright 2011 Shell Global Solutions

 Testing Used Grease

• Most grease tests require two ounces or

more of product to perform.

• Testing of used grease often requires

adaptation of test methods.

Copyright 2011 Shell Global Solutions

 Used Grease Tests
• Appearance
• Water by Crackle Test
• Fourier Transform Infrared (FTIR) Analysis
• Elemental Analysis
• Ferrography / Ferrous Density
• Penetration (½- or ¼-scale)
• Grease Rheometry – test method under development
• Pressure Differential Scanning Calorimetry (PDSC)
• Remaining Antioxidant by Linear Sweep Voltammetry
(RULER)
• SRV (EP)
• SKF Grease Test Kit (TKGT 1)
Copyright 2011 Shell Global Solutions
 Appearance

• Appearance is the most important of all

tests on used grease.
• Appearance consists of:
– Color
– Texture
– Odor
• Photographic Documentation

Copyright 2011 Shell Global Solutions

 Appearance - Color

• The color of the used grease should be

compared to the color of the unused
product.
• Color can indicate proper product
application, contamination, oxidation, etc.

Copyright 2011 Shell Global Solutions

 Appearance - Texture

• The texture of grease can range from

smooth and buttery to rough, stringy,
mealy, fibrous, etc.
• The texture of used grease can indicate
the presence of contaminants (dirt/dust,
wear debris, water, oxidized grease).
• Spreading a thin layer on a white ceramic
tile can be very helpful.
Copyright 2011 Shell Global Solutions
 Appearance - Odor

• Although not technically a part of the

visual appearance of a used grease, the
odor of the product can tell a lot about
how the product was used.
• Odors of oxidation, additive degradation,
or contamination can help to indicate what
further tests should be performed.

Copyright 2011 Shell Global Solutions

 Photographic Documentation

• Photographs of grease samples and

used/failed parts help to document the
samples in as-received condition.
• Photomicrographs show contaminants in
the sample.

Copyright 2011 Shell Global Solutions

 Sample Photographs

Copyright 2011 Shell Global Solutions

 Sample Photographs

Copyright 2011 Shell Global Solutions

 Water by Crackle
• Simple, easy test, very small sample required
• Place grease in a metal or glass dish
• Touch with a hot soldering iron
• Heat on hot plate
• Popping or crackling indicates water
• Water can be detected even when there is no visual
indication of water contamination.
• A trained ear can differentiate between levels of water
contamination.
• For an analytical result, run ASTM D95 Water by
Distillation.

Copyright 2011 Shell Global Solutions

 FTIR Analysis

• Most Useful When Compared Against Unused Grease

• Base Fluid Characteristics
• Thickener Type and Concentration
• Additives and Additive Degradation Products
• Oxidation
• Water and Other Contaminants
• Grease Mixtures
• Fluid and Solid Portions Can Be Separated and Analyzed
• The Most Data with the Smallest Sample
• The Biggest Bang for the Buck
Copyright 2011 Shell Global Solutions
 FTIR Analysis

Copyright 2011 Shell Global Solutions

 FTIR Analysis

Copyright 2011 Shell Global Solutions

 FTIR Analysis

Copyright 2011 Shell Global Solutions

 Elemental Analysis

• Multiple Test Methods:

– Atomic Absorption (AA)
– Inductively Coupled Argon Plasma (ICP)
– Spark Emission Spectroscopy
– X-Ray Spectroscopy
– Ash with Scanning Electron Microscopy with Energy
Dispersive X-Ray Spectroscopy (SEM/EDS)

Copyright 2011 Shell Global Solutions

 Elemental Analysis

• Used to Determine:
– Environmental Contaminants
• Aluminum, Boron, Calcium, Chlorine, Iron,
Potassium, Silicon, Sodium, Titanium
– Wear Metals
• Iron, Copper, Chromium, Aluminum, Silver, Nickel,
Lead, Tin, Titanium, Cadmium, Molybdenum,
Manganese

Copyright 2011 Shell Global Solutions

 Elemental Analysis

• Used to Determine
– Additives
• Calcium, Phosphorus, Zinc, Magnesium, Sulfur,
Barium, Boron, Molybdenum, Lead, Silicon,
Antimony, Chlorine
– Thickeners
• Lithium, Calcium, Sodium, Aluminum, Barium,
Silicon, Titanium

Copyright 2011 Shell Global Solutions

 Ferrography / Ferrous Density
• Analytical Ferrography
– Separation of Particles by Size and Type
– Particle Types:
• Abrasive/Cutting Wear
• Fatigue/Spalling
• Corrosive (Red/Black
Oxides
• Adhesive Wear
• Spheres
– Contaminants
• Ferrous Density
– Concentration of Ferromagnetic Metals
Copyright 2011 Shell Global Solutions
 Analytical Ferrography

• Examples of particle
types that can be
identified with
Analytical Ferrography

Copyright 2011 Shell Global Solutions

 Small-Scale Penetration –
ASTM D1403
• ½-Scale and ¼-Scale Tests
• Requires Smaller Sample
• Less Precise than Full Scale

Copyright 2011 Shell Global Solutions

 Grease Rheometry

• Potential to be Powerful Technique

– Useful for evaluation of in-service greases
• Small sample size (~5 g)
– Test under controlled conditions
• e.g. applied stress, temperature, frequency
• Initial Focus on a Fundamental Test
– Controlled stress-sweep
• Irrecoverable breakdown of thickener structure
• More Complex Methods to Follow

Copyright 2011 Shell Global Solutions

 Pressure Differential Scanning
Calorimetry (PDSC) – ASTM D5483

• Oxidation Stability Test

• Oxidation Induction Time at Specified
Temperature
• Compared to Value for Unused Product

Copyright 2011 Shell Global Solutions

 Remaining Antioxidant by Linear
Sweep Voltammetry – ASTM D7527

• RULER Test
• Used to Detect Phenolic and Aminic
Antioxidants
• Compared to Data for Unused Product
• Used to Calculate Remaining Antioxidant
in Product
• Indicates Remaining Useful Life of Grease

Copyright 2011 Shell Global Solutions

 Extreme Pressure by SRV –
ASTM D5706
• Small Sample Required
• Fast Test Turn-around Time
• Compare to Data for Unused Grease
• Used to Determine Changes in Load
Carrying Characteristics Due to Additive
Degradation or Depletion

Copyright 2011 Shell Global Solutions

 Summary

• Used Grease Samples are Typically Very Small

• Difficult to Obtain Representative Samples
• Most Tests for Unused Grease are Not Suitable
for Use With Used Greases
• Testing of Used Grease Requires Specialized
Tests
• Used Grease Can be Tested Sufficiently Well to
Provide Meaningful Information

Copyright 2011 Shell Global Solutions

 Questions?

Copyright 2011 Shell Global Solutions

 Thank You!
David Turner
Lubricants Technical Advisor
Shell Global Solutions (US) Inc.
3333 Hwy. 6 South, L-117A
Houston, TX 77082 USA
+1 281-544-9214
david.turner@shell.com

Copyright 2011 Shell Global Solutions