USED OIL ANALYSIS

INDIAN OIL CORPORATION

LIMITED
(Marketing Division)
Gujarat State Office
May 2007

SERVO WORLD CLASS LUBRICANTS

SERVO SIGNIFIES
S FOR SERVICE
E FOR EFFICIENCY
R FOR RELIABILITY
V FOR VERSATILITY
O FOR ORIGINALITY

LUBE OIL REQUIREMENTS

DETERGENCY
DISPERSANCY
TBN RETENTION
THERMO - OXIDATIVE
STABILITY
ANTI - WEAR
WATER SHEDDABILITY

REASONS FOR OIL DEGRADATION

AND CONTAMINATION
OXIDATION OF OIL.
LOSS OF ADDITIVE EFFECTIVENESS.
COMBUSTION PRODUCTS AND FUEL DILUTION.
SOOT BUILT UP AND WEAR METALS.
WRONG TOP UP, COOLANT / WATER
CONTAMINATION.

CONDITION MONITORING OF
LUBRICANTS HELPS TO: CHECK QUALITY OF FRESH OILS
CHECK CONDITION OF OIL IN USE / EXTEND
DRAIN

INTERVAL.

ASSESS THE CONDITION OF MACHINE.

ESTABLISH THE DRAIN INTERVAL BY TRIAL
RUN.
REDUCE THE UNSCHEDULED DOWNTIME BY
PREVENTIVE MAINTENANCE.

TESTS FOR CONDITION

MONITORING.

APPEARANCE / COLOR.
WATER CONTENT.
VISCOSITY.
TOTAL ACID NUMBER / TOTAL BASE NUMBER.
WEAR METALS.
FOURIER TRANSFORM INFRARED SPECTROSCOPY.
HEXANE AND TOLUENE INSOLUBLES.
PARTICLE COUNT.
DEMULSIBILITY.
FLASH POINT

USED OIL TESTS AND THEIR SIGNIFICANCE

1.

Appearance
In this procedure the oil samples is placed in narrow glass
container and is visually examined for colour. The results
are reported as clear, hazy cloudy, milky or opaque.
Significance: The appearance of an oil can provide a number
of distinctive clues about oil condition and contamination. A
hazy or cloudy appearance often indicates water
contamination, while a gradual darkening occurs as the oil is
oxidised. Particles as small as 40 microns can be detected
by the unaided eye, providing an indication of gross
particulate contamination.
This test is limited by the
subjective nature of the observer and it cannot be used for
the oils that are dark to begin with.

2.

Water
ASTM D 95 procedure determines water content by
distillation and expresses the results in volume
percent (vol%) Water content can also be
determined as per ASTM D 1744 by reacting the oil
sample with Karl Fischer reagent. This method is
particularly accurate for small quantities of water
and results are express in ppm.
Significance:Water reduces the lubricity of the oil
and leads to corrosion of metal parts. Higher levels
of water may emulsify the oil. In circulating system
water enters from oil cooler leakages. In steam
turbines water can also enter due to condensation of
flue gases.

3.

Kinematic Viscosity
Time taken for a given volume of oil to pass
through a specific size orifice at a given
temperature is measured and is converted into
kinematic viscosity in centistokes.
Significance: This is the most important property.
Used oil viscosity may increase due to oxidation,
ingress of insoluble products or contamination
with higher viscosity products. Viscosity reduces
due to fuel dilution to ingress of low viscosity
products e.g. refrigerants.
Oils incorporating
polymeric
compounds
as
viscosity index
improvers may have viscosity loss due to
permanent shear of VI improvers

4.

Viscosity Index
This is calculated or read from viscosity of the oil
at 40oC and 100oC it is reported in whole number.
Significance: Generally viscosity index of used oils
does not change from original value. Higher or
lower value indicates contamination. Used Engine
oils may show high VI due to fuel dilution.

5.

Flash Point
Flash point of lubricating oils is measured by
ASTM D 93 (PMCC) procedure as they may
contain lighter fractions. The test oil is heated
in the prescribed apparatus and the oil
temperature at which vapour flashes in the
presence of pilot flame is noted. Values are
expressed in oC.
Significance:
Reduced flash point values
indicate presence of volatile products like
solvents of fuel. Cracking of oil also reduces
flash point.
Higher flash point indicates
admixture with wrong grade of oil

6.

Total Base Number

ASTM D 2896 procedure determines the level of
alkalinity in an oil sample by measuring the change
in electrical conductivity during titration with
Perchioric Acid. The results are expressed as mg
KOH/g.
Significance: Most motor oils are formulated with a
variety of additives that enhance lubricity, retard
oxidation, improve viscosity characteristics and
pour point and reduce the tendency for sludge and
deposit formation.
The level of additives is
determined by measuring the TBN. With use TBN
value decreases from new oil value.
When it
reaches a critical limit oil requires change

7.

Total Acid Number

ASTM D 974 procedure determines the level of acidity by mixing
in an indicator solution and then adding potassium hydroxide
(KOH) until solution changes colour. Some samples may be
too dark to use a colour in indicator and for such cases ASTM D
664 procedure measures the change in electrical conductivity
as the KOH is added. The acidity is expressed as mg KOH/g.
Significance: As oils oxidise they form acidic by-products
which can be corrosive to metal components. The greater the
oil degradation, higher would be the level of corrosive acids
and greater the danger of components failure. Some oils, like
hydraulic fluids, have additives which are themselves acidic.
For such cases, the most meaningful measure is the change in
acidity from new oil value. TAN should not be used as the sole
criterion for oil deterioration due to oxidation and other
properties such as viscosity, insolubles and sludge contents
must also be considered.

8.

Hexane & Toluene Insolubles

ASTM D 893 procedure measures quantum of insolubles
remaining undissolved in Hexane solvent after centrifuging.
Insoluble matter is further dissolved in toluene solvent and
centrifuged and insoluble matter is weighed. Insolubles are
reported as percent mass.
Significance: Hexane insoluble products, consists of oxidation
resins plus extraneous matter like carbon, soot, wear particles,
dust and dirt etc. Toluene dissolves the oil oxidation products
and therefore Toluene insolubles consists of only extraneous
matter. Difference between Hexane Insolubles and Tolune
insolubles indicates amount of oil oxidation products. Low
Hexane insolubles indicate that the oil is in good condition. If
Hexane insolubles are high, the subsequent Toluene insolubles
indicate whether contamination is due to oil oxidation or
extraneous matters or both.

9.

Sediments
In this test the oil sample is kept in tumbler and is washed with a
solvent in the specified apparatus. The sediments so collected are
weighed and results are reported as percent mass.
Significance:
A.
Less than 0.05% by volume of sediment is
reported as trace
B.
No more than a trace of sediment indicates
Relatively little oxidation or no
contamination and the product being in
satisfactory condition
The purification system is functioning
properly
C.
More than a trace (0.05%) of sediment indicates:
Oxidation, accompanied by increased neutratisation
number and viscosity.
The presence of inorganic impurities (e.g.metal particles,
dust, dirt, etc.)when accompanied by a high ash value.
The purification system is not functioning properly.

The nature of sediments is determined by their

solubility on chloroform.
If the sediments are
soluble in chloroform the presence of oxidised oil
and/or metalic sops is indicated. If the sediment is
completely or even partially insoluble in the
chloroform, further analytical work is required to
determine the exact nature. Where more than a
trace of sediment is reported, efforts should be
made to correct the condition

10

Rust Test:
The procedure consists of two parts-Procedure A:
using distilled water and Procedure B: using
synthetic sea water. Most new lubricants are
formulated to pass either Procedure a or B.
Premium quality turbine oils, gear oils and
hydraulic fluids are formulated to pass procedure
B. In this method the oil to be tested is mixed
with 10% distilled water or synthetic sea water
and a polished grade 1018 carbon steel specimen
is inserted in the solution and system is kept at
60oC for 12 hrs. or 24 hrs. The steel specimen is
observed for rusting. Results are reported as
Pass or Fail.

Significance
Lubricating oil in turbine or other system
incorporating oil cooling often gets contaminated
with water, resulting in rust Particles of rust in the
oil can act as catalysts and tend to increase the
rate of oil oxidation.
Rust particles being
abrasive can also cause wear and clogging of
service valves. The used oil in circulation must
show pass value under this test to be fit for
further use.

11.

Demulsibility:
40 ml sample of oil and 40 ml of distilled water are
mixed in a 100 ml cylinder and kept at 54oC. The
time taken for emulsion to reduce to 3 ml or less
is recorded in steps, of 5 minutes.
If the emulsion is more than 3 ml after one hour
the test is discontinued and the remaining amount
1(in ml) of oil, water and emulsion are recorded.
Significance: Water promotes rusting of ferrous
parts and accelerates oxidation of the oil for
effective removal of water the oil must have good
demulsibility characteristics.

12.

Foaming:
The test oil is kept at 23.9oC temperature and air
is passed through the oil sample for 5 minutes.
The amount of foam generated and the time taken
by foam to collapse is noted. A fresh sample of
the oil is tested at 93.3oC. In the 3rd stage, after
carrying out the test at 93.3oC. The results are
reported as volume of foram in ml, at the end of
blowing period and at the end of setting period for
3 different test temperatures. The foam volume at
the end of blowing period is termed as the
foaming tendency of the oil, while the foram
volume at the end of blowing period is termed as
the foaming tendency of the oil, while the form
volume at the end of the setting period is termed
as the stability of the foam.

Significance: Foaming in a circulating oil system is a

serious service condition that may interface with
satisfactory system performance and even lead to
mechanical damages. Foaming consists of bubbles
that rise quickly to the surface of the oil and it should
be distinguished from air entrainment which consists
of slow rising bubbles dispersed throughout the oil.
Foaming can be both system oriented and oil related.
Excessive turbulence of the oil or air leakage in the oil
flow may lead to foaming. Trace contamination of the
lubricant by surface active materials such as rust
preventives and detergents can also cause foaming.
Foaming in an industrial oil is undesirable because
the foam may overflow the reservoir and create a
nuisance.

The nature of sediments is determined by their

solubility on chloroform.
If the sediments are
soluble in chloroform the presence of oxidized oil
and/or metallic sops is indicated. If the sediment is
completely or even partially insoluble in the
chloroform, further analytical work is required to
determine the exact nature. Where more than a
trace of sediment is reported, efforts should be
made to correct the condition

13.

Trace Metals:

Emission spectroscopy and atomic absorption are two

common methods for determining trace metals in used
or new lubricating oils. Both these techniques require
small quantity of oil sample. Results are reported in
parts per million or parts per billion concentration of
inorganic metals in the oil sample.
Significance: New oils contain metallic additives and the
quantum of these additives can be determined by
concentration of trace metals like zink, calcium,
phosphorus, etc. Trace metal analysis in used oil
indicates depletion of additives and wear metal particles
concentration. The analysis of wear metal particles can
be used for monitoring condition of the equipment. The
following is the list of elements generally found in used
industrial and engine oils and their sources

CANNON AUTOMATIC VISCOMETER

CAUSES , EFFECTS & RECOMMENDATION FOR VISCOSITY

CHANGES.
CAUSES

EFFECTS

RECOMMENDATIONS

HIGH VISCOSITY
Contamination soot/solids
Oxidative degradation.
Leaking headgasket.
Water Ingress
Over extended oil drain.
High operating temperature.
Incorrect oil grade or type.
Cross contamination.

Restricted oil flow.

Machine overheating.
Accelerated wear.
Impeded low
temperature operation

Check fuel pipes and

injector calibration.
Check for correct oil
grade / type.
Check for correct operating
temperature.
Check for leaking injector.
Check operating condition.
Change oil and filters.
Evaluate equipment
suitability for use.

Increased friction

LOW VISCOSITY
Polymer shearing
(multigrade oils)
Fuel dilution.
Incorrect oil grade or type.
Cross contamination

Machine overheheating
Machine overheating.
Metal to metal contact.
Accelerated wear.
Increased leakage

DIRECT READING EMMISSION

SPECTROMETER

DIRECT READING EMMISSION SPECTROMETER

IT IS USED FOR.
DEPLETION OF ADDITIVES IN USED OILS.
WEAR ELEMENTS / CONTAMINANTS BUILD UP.
TO IDENTIFY COOLANT/ WATER
CONTAMINATION.
QUALITY CHECK OF FRESH OILS.

RESULT OF WEAR-PARTICULATE
CONTAMINATION

Abrasion.
Cavitation and Erosion.
Corrosion
Adhesion
Surface Fatigue
Conaminant Monitoring - Predictive Maintenance

ELEMENT / CONTAMINANTS & THEIR SOURCES

ELEMENT

TYPICAL SOURCE

IRON
CHROMIUM
LEAD
COPPER
TIN
ALUMINIUM
NICKEL
SILICON
ZINC
VANADIUM
BORON
POTASSIUM

CYLINDER,RUST,CRANKSHAFT,WATER.
CYLINDER,RING,COOLANT,CRANKSHAFT
GASOLENE,BEARING,GREASE,PAINT.
BEARING,BUSHING,BRONZE.
BEARING,SOLDER,COOLERS.
DIRT, DEPOSITS.
SHAFT,GEARS,RINGS,TURBINE COMPONENTS.
DEFOAMANTS,DIRT.
ADDITIVES,BEARINGS,PLATINGS.
FUEL,CATALYSTS,TURBINE BLADES,VALVES.
COOLANTS,ADDITIVES,SEA WATER.
COOLANTS,ADDITIVES,DIRT.

FUEL DILUTION
Amount of Dilution
Viscosity Effect
5% SAE 3020
7% SAE 3010
Change oil when fuel dilution exceeds 2%
Reduces lubrication and dilutes additives
Tests for fuel dilution: Viscosity,FTIR,Flash
Point(ASTM D-93), Gas Chromatography(ASTM
D3524), Steam Distillation.

CAUSES OF SOOT BUILD UP

Incomplete combustion
Low compression
High fuel /air ratio
Improper scavenge operation
Excessive ring wear / blow by.
Tests for Soot:-Toluene Insol.(D893), Membrane
Filtration, TGA.

Plugged air filter.

Excessive idling.
Cool engine temperatures.
Poor fuel nozzle.
Defective turbo operation.

MAXIMUM CONTAMINATION LIMITS(BASED ON A 100 ML SAMPLE)

MAXIMUM CONTAMINATION LIMITS(BASED ON A 100 ML SAMPLE)

SAMPLING FREQUENCY
EQUIPMENT
Diesel engines.
Hydraulics
Gas Turbine industrial
Steam turbines.
Air/gas compressors
Gear Boxes-high speed
Gear boxes-low speed
Marine /DG Set
Stationary engines

HOURS
150-300
200
500
500
500
300
1000
500
1000