Laboratory Grease Analysis with Grease
Thief Sampling & Analysis System
• Grease Thief Die Extrusion
• Analex fdM+ Ferrous Debris
• Metal Spectroscopy Grease
Consistency
Anti-oxidants
• RULER
• FT‐IR Comparative
FTIR
Offsite
Grease Analytical
Ferrography
Tests
• Analytical Ferrography
• Rheology
Metals Patch
Spectroscopy Microscopy
Grease
Rheology
Prep for Analysis
• When grease is tested for consistency, it can
be extruded onto sample substrates:
– IR Card for FTIR
– Substrate for weighing and dissolution in RULER
vial
– Substrate for weighing and dissolution for
spectroscopy; same dissolved grease can be used
for Ferrography/MicroPatch
Sample Handling and Preservation
• Sampling Procedures: ASTM Standard Practice
D7718
• Use proper PPE
• Instrumentation
– Wipe down between runs
– Do not reuse Extrusion Dies or Grease Thieves
(GT)
Analysis Techniques
Sample is received. fdM+ is run Grease Thief Analyzer is performed and substrate is made
Two strips are used to make One Strip is used One Strip is Dissolved in Green
a dilution to run RDE/ICP. for FT-IR. RULER solution to run RULER.
Wear Monitoring with the ANALEX
fdM+
• Hall effect type sensor to
determine the amount of
ferrous debris present in the
sample.
• Instrument has calibration
standards for Grease Thief.
• The instrument measures the
entire sample which is
important due to the non‐
homogenous nature of grease.
Wear Monitoring Method Comparison
• Sample was taken in grease sampler
• Extruded sample was weighed and dissolved for
direct reading ferrography
• Results were normalized to 0.1 gram grease
• Full sampler analyzed by ferrous density
instrument (Hall effect sensor) for ppm Fe result
• Quantity of grease in sampler weighed and tared,
and result in ppm normalized to 1.0 gram grease
Standard Relative Standard
Method Average
Deviation Deviation
fdM+ 277 ppm 7 2.53
DR- 205 46 22.44
RDE 57 ppm 16 28.07
Grease Thief Die Extrusion Test
• This instrument detects changes in the consistency of a
grease.
• It is sensitive to the presence of hard particles, seen as
spikes in the data, and hardened chunks of grease, seen
as broad peaks in the graph.
• This test only requires one gram of grease.
• Grease Thief Index (GTI) calculates the deviation in
percent of the force of the sample compared to that of
the baseline. A GTI of 100 shows a perfect match to the
baseline.
Die extrusion and sample preparation
• Grease extruded through die to create ribbon on substrate
• Load profile at varying speeds developed for consistency evaluation
• Sample prepared for subsequent analyses
Predicted Response Graph
• Average stable load value
after speed change related
to NLGI grade, or
penetration values
• Rapid speed changes used
to leverage non‐Newtonian
response
• Critical areas expected
immediately after speed
change; possible data rich
regions to characterize
rheology, oil shear,
“dryness”, etc.
Grease Thief Analysis Profiles
Hardened Sample
Normal Profile
1000
1000
900
900
800 800
Force (grams)
Force (grams)
700 700
600 600
500 500
400 400
300 300
200 200
100
GTI = 89 100
GTI = 183
0 0
272 372 472 572 672 772 872 320 420 520 620 720 820
Sample Baseline
sample baseline
Softened Grease Sample with Hard Particles
1000 1400
900
1200
800
Force (grams)
Force (grams)
700 1000
600
800
500
600
400
300
GTI = 31 400
200 GTI = 76
200
100
0 0
272 372 472 572 672 772 300 400 500 600 700 800
Sample Baseline Sample Baseline
Actual Load Response Graphs
Consistency Testing
Standard Laboratory Tests
• FT‐IR – Takes a fingerprint of the grease. Helps
determine if mixing is present. It is also used to
determine the presence and origin of unknown
contaminants and oxidation.
• RULER – Measures the amount of anti‐oxidant
remaining in the grease.
• Metal Spectroscopy – RDE/ICP/XRF determines the
wear metals, additive metals and thickener metals
used in the grease formulation. This test also aids in
the detecting mixing of greases.
• Optical Spectroscopy – Uses visual color absorbance
to evaluate degradation and potential mixing.
FTIR Analysis
Prep for Analysis
Linear Sweep Voltammetry (RULER)
analysis for grease
• Preparation of thin‐
film substrate
streamlines and
standardizes analysis
• Additive levels
normalized to mass of
grease
Linear Sweep Voltammetry
• Samples from similar coal
crushers, same time in service
• Both have an adequate
remaining anti‐oxidant level to
protect grease from oxidation
• Lower sample shows more
rapid degradation of anti‐
oxidants, due to higher
temperatures, contaminants,
or other oxidation stressors.
• Differences in time of service
or relubrication quantities or
effectiveness could also affect
anti‐oxidant amount
Optical Spectroscopy Cell
In‐Service Spectrum
0.6000
0.5000
New Fluid in‐service Fluid
0.4000
0.3000
Mobilith SHC 220
0.2000
0.1000
0.0000
400
413
426
439
452
465
478
491
504
517
530
543
556
569
582
595
608
621
634
647
660
673
686
699
50:50 Mixture
New Lubricant to End of Life
0.50
0.45
0.40
New Fluid
0.35
Transmission
In-Service Fluid
0.30
End of Life Fluid
0.25
0.20
0.15
0.10
0.05
0.00
400 450 500 550 600 650 700
Wavelength (nm)
New: Mobil XHP 222 S, In-service: Used Mobil XHP 222, EOT: Used
Unirex N2 (both were the same at end of life).
Chemometric Techniques
• Evaluate particulate contamination of new and in‐
service greases
• Coal dust, other known and common contaminants
• Establishing contaminant level targets
Carbon Residue Experiment
• Carbon residue CIE and L* Vs. % Carbon Residue
used to make a 1% 70
by mass mixture. 65
• Dilutions made to y = 564.03x + 56.949
R² = 0.969
prepare 9 60
additional samples.
55
• Extruded samples y = -640.87x + 58.179
R² = 0.9534
onto substrates. 50
• Analyzed samples 45
with the i‐Lab
using the optical 40
0.00% 0.20% 0.40% 0.60% 0.80% 1.00%
spectroscopy box. Carbon Residue (percent mass)
CIE ∆E L*
Carbon Residue Experiment
Carbon Residue Experiment 2 Visual Spectra Comparison
0.7
0.6
0.5
Transmittance
0.4
0.3
0.2
0.1
0
400 450 500 550 600 650 700
wavelength (nm)
1.00% 0.90% 0.80% 0.70% 0.60% 0.50% 0.40%
0.30% 0.20% 0.10% 0.00%
Advanced Laboratory Testing
• Rheometric Analysis is a • Analytical Ferrography
newer technique that microscopic technique
utilizes a rheometer to used in oil and grease
analyze the physical analysis. It is used to –
properties of a grease. – Discover the origins of
These properties are – the wear.
– Resistance to flow – The size of the particles.
(pumpability) – Detect signs of acid
– Consistency corrosion.
– Recoverable Compliance
(tunneling)
Rheometer testing
• Work by Nolan and Sivik to evaluate grease
properties with rheometer
• Bryan Johnson published method for
correlating penetration to rheometer
• German DIN draft method
• Yield stress point and equilibrium recoverable
compliance
• Measuring flow point and elastic recoil
Rheometer Consistency Testing
Elasticity or Recoverable Compliance
Consistency Testing
New fresh grease G’= 18,260Pa
Suspected Mixture G’=10,510Pa
G’ is 57% of new
Ferrographic and Micro‐Patch
inspections
Ferrographic and Micro‐Patch
inspections
• Analytical ferrography more difficult than oil; may
require special “fixer” mixtures
• Patch can be clouded by residual grease particles,
but can be more effective at finding non‐ferrous
Wind Turbine grease sampling and
analysis
• 2‐year project conducted with DONG Energy and
Vattenfall, two largest offshore wind operators in the
world
• Dr. Kim Esbensen, internationally recognized expert in
Theory of Sampling (TOS), Denmark
• Rich Wurzbach, MRG Labs, inventor of Grease Thief
• Systematic evaluation of grease heterogeneity,
sampling methodology, and analysis validity and
repeatability for wind turbine main bearings in on‐
shore and off‐shore applications
• Results published at OilDoc, LUBMAT, and AWEA
•Fundamental Sampling Principle
–Using the Grease Thief
•Representative sampling
–Thorough characterization of the heterogeneity of
grease in main bearings
Test parameters of Grease
•For the heterogeneity characterization of
grease in main bearings of wind turbines the
following parameters were used:
–Consistency and flow characteristics
–Ferromagnetic iron (Hall‐effect sensor)
–Wear metals
–Particle characterization (size & distribution)
–Residual oil in grease
–Antioxidants
Heterogeneity characterization –
Ferromagnetic iron
• Sampling of grease while draining the main bearing through
the drain plug
• 27 increments collected (each sample approximately 20
grams)
On site sampling
20000
18000
I ro n (F d M P l u s )
16000
14000
12000
10000
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27
Sample no
