When should I change

my Oil?
Moussa ZIDOUNE, PhD, Chemist

Training Session, May 2011

Agenda
Lubricants
Test Methods
Reports and
Interpretation
Conclusion

Base Oils General Classification

Mineral Oils: products of the distillation of crude petroleum, consiting of
hydrocarbon chains:
Paraffinic
Naphtenic
Aromatic

Synthetic Oils: oils made by chemical synthesis:

Polyalphaolefins (PAO)
Polyglycols (PAG)
Ester oils
Silicones

Semi-synthetic: blends of mineral oils with synthetic base oils

Vegetable Oils: made of soja, corn, castor, canola, cotton seed

Classification of Lubricants by
Additives
Additives are substances formulated for the
improvement of the anti-friction, chemical and physical
properties of base oils (mineral, synthetic, vegetable or
animal), which results in enhancing the lubricant
performance and extending the useful life of
equipments.

Additives can make up to 30% of the

lubricant.

 Friction modifiers
Anti-wear
Extreme pressure (EP)
Anti-rust and corrosion inhibitors
Anti-oxidants
Detergents
Dispersants
Pour point depressants
Viscosity index enhancers
Anti-foaming agents

Classification of Lubricants by application

Engine oils
Gear oils
Hydraulic oils
Compressor oils
Transformer oils (insulating oils)
Turbine oils
Cutting fluids (coolants)

Engine Oils
Functions of engine oil:
Provision of stable oil film between sliding
surfaces
Provision of reliable engine operation in a wide
temperature range.
Rust/corrosion protection of the engine parts
Cleaning sludge from the engine parts
Sealing piston ring - cylinder gap
Prevention of foaming
Cooling the engine parts

Hydraulic Oils
Characteristics and properties
Thermal and chemical stability
Low compressibility
Hydraulic stability
Good lubrication
Low foaming
Emulsion capacity

Benefits of Oil Analysis

Reduction in maintenance costs

Reduction in unscheduled downtime
Reduction in unscheduled maintenance
Reduction in machine power consumption
Effective maintenance scheduling
Improved equipment reliability.
Maximization of oil change out intervals.
Minimization of installation errors.
Increase in equipment availability
Reduction in disposal cost

Oil Analysis allows detection of:

Contamination

Dirt and dust

Water
Glycol
Fuel
Soot
Sulfates and nitrates
Particles

Degradation of the lubricant

Kinematic viscosity (VIS)
Oxidation (FTIR)
Acid number (AN)
Base number (BN)

Wear

Inductively Coupled Plasma (ICP)

Direct Reading Ferrography (DR)
Analytical Ferrography (AF)
Filter Debris Analysis (PT)

Test Methods

 SP Spectroscopy
VIS Viscosity
FTIR Infrared Analysis

FU- Fuel
FP Flash Point
FIRE Fire Point

TAN Total Acid Number

TBN Total Base Number

GYL Glycol
Water -Tests

PC Particle count
DR Direct reading
PT Filter Analysis
AF Analytical Ferrography VCT Varnish Test

Machine and Lubricant Condition

MACHINERY

SP

LUBRICANTS

AF
DR
PC

PC
DR

FTIR VIS
TAN TBN
Water, FU

SP - Analytical Spectroscopy
Detects 22 elements (Particles <7 microns in size)
Aluminum Barium Boron Cadmium Calcium Chrome Copper Iron
Lead Magnesium Manganese Molybdenum Nickel Potassium
Phosphorous Silicium Silver Sodium Tin Titanium Vanadium Zinc

Wear Metals
Contamination
- Boron, Sodium, Silicium, Potassium, Aluminum

Additives
- Calcium, Phosphorus, Zinc, Magnesium, Barium

VIS - Viscosity
Measures the resistance to flow
Measured in centiStokes (cSt)
40 C and/or 100 C
Affected by:
Oxidation
Contamination
Change oil if the limit is > 20%, and
Monitor trend if > 10%!

FTIR Infrared Analysis

Fingerprint of the lubricant
Soot Level
Oil Degradation
Oxidation
Nitrates
Sulfates

Contamination

Glycol
Water
Fuel

Water &
glycol

Absorbance

Thickening Oil

Degradation
Products

New oil

Oxidation

Additives Level
400
350
300
250
20
150
0
0
0
0
00
Mineral or Synthetic Base Oil Wavelength (cm 0)
-1

100
0

Total Acid Number(TAN) Total Base Number

(TBN), ASTM D974 & ASTM D4739
TAN indicates oil oxidation or contamination by
an acidic product.
Acid number increases with oxidation
Recommended for all industrial equipment

TBN measures the alkaline content of oil.

Abnormal reduction indicates reduced acid neutralizing capacity.
Recommended for engines

Effects of Water on Oil

Causes hydrolisis and oxidation
Generates acids
Thickening
Varnish and sludge
Contributes to foaming and emulsion

Effects of Water Contamination on the

Machine
Water accelerates machine deterioration
Corrosion: water in oil confers their maximum
destruction potential to acids
Loss of lubricating film, cavitation, lower
filtration capacity and blocks valves.

Bearing wear due to water

contamination

Water Detection Methods

Hot Plate Test - Semi-quantitative

FTIR (infrared) - Qualitative
Spectroscopy Indicative
Karl Fischer Coulometric titration Quantitative
Distillation, ASTM D95 - Quantitative

Hot Plate Detection Method

0.0%,

0.1%

1.0%

2.0%

The hot plate test is very effective in detecting

water in quantities equal to or higher than 0.1%
(1000 ppm or more).
Results: 0.0%, 0.1%, 1.0%, 2.0%, 5%

FTIR Detection Method

Degradation Products
(nitrate-sulfate)
3.5

Water & glycol

Oil Thickening

3.0

2.5

New Oil

2.0

1.5

Oxidation

1.0

0.5

4000

3500

3000

2500

2000

Wavelength (cm-1)

1500

1000

Spectroscopy
Presence of boron, B
Presence of sodium, Na
Presence of potassium, K

Distillation Method
Cooler

Quantitative Method for

High Concentration (5% -100%)

Water

Heating plate

KF - Karl Fisher ASTM D4928

Applicable when and where water
contamination level is critical and must
be kept very low.

Both equipment and oil can accept a certain amount of water

Result is given in percent (ex: 0.1% =

1000 ppm).

Glycol Contamination
Antifreeze
Glycol and water are the main constituents (50/50) of
antifreeze or coolant liquids.
Ethylene Glycol (High heath transfer)
Propylene Glycol (More toxic, less popular)
Additives: Phosphates, borates, molybdates,
silicates, nitrates, potassium ...etc

Effects of Glycol

Oil thickening, change in viscosity

Emulsion and gels, dispersion
Acid formation
Precipitation of additives
Lower oil debit
Filter degradation
Bad lubrification

Glycol Detection Methods

FTIR Detection
Degradation Products
(nitrate-sulfate)

3.5

Water & glycol

Oil Thickening

3.0

2.5

New Oil
o
x
y
d
a
ti
o
n

2.0
1.5

1.0

0.5

4000

3500

3000

2500

2000

Wave length (cm-1)

1500

1000

Detection by Spectroscopy
Presence of Boron, B
Presence of sodium, Na
Presence of potassium, K
Presence of silicium, Si

Detection by ASTM D2982 Method

Colorimetric method
A HCL solution is added to oil to oxidize glycol
The reaction produces aldehyde
Aldehyde reacts alternatively with a reactant, producing
a positive color change from colorless to pink / to
purple
The darker the color, the more glycol there is
Results: 0.01%, 0.05% and 1 %

Detection by GC ASTM D4291 Method

This method is the most precise, although more
expensive and more time consuming than others.
The most widely used GC procedure is ASTM 4291.
First you must extract glycol
Extract is then injected into the GC where polar
components are separated and detected on a
chromatogram.

Fuel Contamination
FU - percent of unburned diesel or gasoline
present in engine

1.
2.
3.
4.

Fuel Dilution ASTM D3828

FTIR Detection
Detection by Flash Point
GC, ASTM D Detection is the most
precise and most expensive method.
5. The most currently used GC method
is ASTM 3524

FP Flash Point ASTM D92

FIRE Fire Point ASTM D92

Oil

FP - Temperature at which the lubricant flashes

when exposed to an open flame
FIRE - Temperature at which the lubricant
continues to burn when exposed to an open flame

Oil

CLP Cloud Point ASTM D97

PP Pour Point ASTM D97

CLP - Temperature at which crystals of paraffin wax

precipitate from solution to obstruct filtration
systems.
PP - Temperature at which the fuel or oil is not
moving (immobilized) once at an angle of 90
degrees to a horizontal surface.

PC Particle Counting
Recommended on all pieces of
equipment requiring filtration
Cleanliness level expressed in ISO
4406 (1999) or NAS 1638 codes
Dimensions () and quantity of the
particles
Water particles are also counted
Evaporation may be used to eliminate part of this
water for a better particle counting.

Code ISO 4406:1999

17/14/13
6

14

ISO 4406:1999
Particles by ml
More than

Up to

Scale

160,000

320,000

25

80,000

160,000

24

40,000

80,000

23

20,000

40,000

22

10,000

20,000

21

5,000

10,000

20

2,500

5,000

19

1,300

2,500

18

640

1,300

17

320

640

16

160

320

15

80

160

14

40

80

13

20

40

12

10

20

11

10

10

2.5

1.3

2.5

0.64

1.3

ISO 4406

NAS 1638

23/21/18

12

22/20/18

--

22/20/17

11

22/20/16

--

21/19/16

10

20/18/15

19/17/14

18/16/13

17/15/12

16/14/12

--

16/14/11

15/13/10

14/12/9

13/11/8

12/10/8

--

12/10/7

12/10/6

--

Comparison between ISO 4406 & NAS

1638 Cleanliness codes

DR Direct Reading
Quantitative Ferrography
Recommended for gearboxes, differentials
and screw compressors
Detects metallic, nonmetallic particles,
contaminants included
Indicates changes in wear rate and severity

AF Analytical Ferrography
In-depth DR
Type of wear
Detection of large particles
Degradation products by
oxidation in suspension
Recommended systematically
when particles are detected

Wear Particles - Debris

By abrasion

Slicing

Copper Alloy

Black Oxides

Red Oxides

Particle Quantifier, PQ
Sensitive Magnetometer - measures the
mass of ferrous debris in the sample in PQ
index.
The PQ index test is quantitative
Recommended for motor oils

Interpretation of PQ results
When iron is high and PQ is low ~> small
particles
When iron and PQ are high ~> small
particles
When PQ is high and iron is low ~> large
particles

Analex PQA

Questions

Varnish
Varnish is a thin, oil-insoluble layer of oil-degradation
residues and by-products that develops over time on
the internal surfaces of lubricated equipment. This can
even occur on well-maintained machines with clean
lubricants.

Oxidation

Causes

Thermal Degradation
Factors: air, heath, water; contamination, radiation,
additive degradation, etc.

How do we Measure Varnish?

Varnish formation potential is measured by :
quantitative spectrophotometric analysis (QSA)
Contaminant, sub-product evaluation method based
on the extraction by disssolution of insoluble
contaminants, through amembrane, measured in
CIE_dE, on a scale of 1 to 100.
The higher CIE_dE is, the higher the proportion of
varnish in the oil.

Varnish Results
NORMAL
< 15

MONITOR

MARGINAL

15 ~ 30

30 ~ 40

CIE_dE Results on a 1 100 scale

Photo of membrane

CRITICAL
> 40

PT Filter Analysis
Used in the aviation industry
Indicates the type of wear particles
Dissolution and filtration of magnetic particles

Action!!
Change oil if viscosity is 20% of initial
value
Change oil if fuel has been detected and
low viscosity
Change oil if glycol has been detected

Action !!
Filter oil if code is higher than recommended
Inspect machine if wear is severe
Proceed to AF test if volume of large particles is
high
Eliminate the source of water infiltration
Monitor color and odor of oil, oxidation index
Eliminate varnish if detected

Test Packages

ENGINES
TESTS
COMPLMENTAIRE
S

MOBFTV

MOBPLUS

CODE

SP
FTIR
VIS100
FU
HP
COPOF

SP
FTIR
VIS100

TBN
FU
HP

COPOF

SP
FTIR
VIS40
VIS100

MENGP

VI

GCF

PQ
HP

COPOF

DESCRIPTION

ANALYSE SPECTROMTRIQUE ICP

ANALYSE INFRAROUGE... FOURIER
VISCOSIT 100 C
DILUTION DU CARBURANT
TEST DE CRPITEMENT
COULEUR,ODEUR,CLART,PRCIPIT,
MOUSSE

ANALYSE SPECTROMTRIQUE ICP

ANALYSE INFRAROUGE... FOURIER
VISCOSIT 100 C
INDICE D'ALCALINIT
DILUTION DU CARBURANT
TEST DE CRPITEMENT
COULEUR,ODEUR,CLART,PRCIPIT,
MOUSSE

ANALYSE SPECTROMTRIQUE ICP

ANALYSE INFRAROUGE... FOURIER
VISCOSIT 40 C
VISCOSIT 100 C
INDICE DE VISCOSIT
(VIS40+VIS100)
CHROMATOGRAPHIE EN PHASE
GAZEUSE CARBURANT
INDICE DE QUANTIFICATION DES
PARTICULES
TEST DE CRPITEMENT
COULEUR,ODEUR,CLART,PRCIPIT,
MOUSSE

MTHODE

ASTM D5185
JOAP

QUANTIT
DHUILE
REQUISE

CALENDRIE
R

ASTM D445
ASTM D3828
PMC

100ml

MENSUEL

PMC

ASTM D5185
JOAP
ASTM D445

ASTM D4739
ASTM D3828
PMC

100ml

MENSUEL

PMC

ASTM D5185
JOAP
ASTM D445
ASTM D445

ASTM D2270
ASTM D3524, ASTM
D3525

100ml

MENSUEL

PMC
PMC

PMC

HYDRAULIQUE
Pompes hydrauliques, Valves hydrauliques, Actionneurs hydrauliques

CODE DES TESTS

COMBINS

PRAN

CODE
SP
FTIR
VIS40
PC

VISCOSIT 40 C
COMPTAGE DE PARTICULES
COULEUR,ODEUR,CLART,PRCIPIT,
COPOF MOUSSE

SP
ANALYSE SPECTROMTRIQUE ICP
FTIR
ANALYSE INFRAROUGE FOURIER
VIS40
VISCOSIT 40 C

PRANP

PC

TAN
KF

DESCRIPTION
ANALYSE SPECTROMTRIQUE ICP
ANALYSE INFRAROUGE FOURIER

COMPTAGE DE PARTICULES

INDICE DACIDIT
TITRATION DEAU DE KARL FISCHER
COULEUR,ODEUR,CLART,PRCIPIT,
COPOF MOUSSE

MTHODE
ASTM D5185
JOAP

QUANTIT
DHUILE REQUISE

CALENDAR

ASTM D445
ISO 4406

100ml

MENSUEL

PMC

ASTM D5185
JOAP
ASTM D445

ISO 4406
ASTM D974,ASTM
D664
ASTM D4928

100ml

MENSUEL

PMC

BOTE ENGRENAGE, DIFFERENTIEL & COMPRESSEUR

CODE des TESTS
COMBINS

CODE
SP
FTIR

DESCRIPTION
ANALYSE SPECTROMTRIQUE ICP
ANALYSE INFRAROUGE FOURIER

VIS40
DR

VISCOSIT 40 C
LECTURE DIRECTE

COULEUR,ODEUR,CLART,PRECIPIT,MO
COPOF USSE

SP
ANALYSE SPECTROMTRIQUE ICP
FTIR
ANALYSE INFRAROUGE FOURIER
VIS40 VISCOSIT 40 C

DROT

DROTP

DR
KF

LECTURE DIRECTE
TITRATION DEAU DE KARL FISCHER

TAN

INDICE DACIDIT

COULEUR,ODEUR,CLART,PRECIPIT,MO
COPOF USSE

MTHODE
ASTM D5185
JOAP

QUANTIT
DHUILE REQUISE CALENDRIER

ASTM D445
PMC

100ml

MENSUEL

PMC

ASTM D5185
JOAP
ASTM D445

PMC
ASTM D4928
ASTM D974,ASTM
D664

100ml

MENSUEL

PMC

GRAISSE
Roulements, Compresseurs, Diffrentiel,
Bote engrenages, Transmission, Turbine
CODE des TESTS
COMBINS

CODE

GRS

SP

GRSPQ

GRS

PQ

DESCRIPTION
ANALYSE SPECTROMTRIQUE

ANALYSE SPECTROMTRIQUE ICP

INDICE DE QUANTIFICATION DES
PARTICULES

MTHODE

QUANTIT
DHUILE REQUISE CALENDRIER

PMC

2g

MENSUEL

PMC

10g

MENSUEL

PMC

VERNIS
Compresseurs, Botes engrenages, Hydraulique, Turbines

CODE des TESTS

COMBINS

CODE
QSA

VBT

GAF

DESCRIPTION
ANALYSE SPECTROPHOTOMTRIQUE
QUANTITATIVE
ANALYSE GRAVIMTRIQUE (FILTRATION)

COPOF COULEUR,ODEUR,CLART,PRCIPIT,MOUSSE

MTHODE

QUANTIT
DHUILE CALENDRIE
REQUISE
R

PMC

PMC

200 ml

TRIMESTRIEL

PMC

Aviation
Metal filter analysis
Patch test (PT)
Chip test when recommended

Aviation Hydraulic Fluid

Spectrometric wear metal check (ASTM
5185)
Viscosity , ASTM D 445
Acidity (TAN)
Water content (KF)
Particle count, (NAS 1638 / ISO4406)

Test Reports

Sample Report

Sample Report

Sample Report

Sample Report

Sample Report

Sample Report

QUESTION
S