Chemical Inspection

(Oil/Lube Analysis)

1
Lubricant History, Formation & Functions

Role of Additives

Three Components of Tribology

Fluid Properties Analysis

Contamination Analysis

Wear Debris Analysis

Oil handling & Storage

Oil Sampling
 Definition of Lubricant

A lubricant is a substance interposed between

two surfaces in relative motion for the
purpose of reducing the friction and wear
between them.

3
 History of Lubricants

The recorded use of lubricants dates back to almost to the birth of

civilization, with early historical developments being concerned
1st stage with the use of fats/oils of animal or vegetable origin in
transportation or machinery. Ancient inscriptions dating back to
1400 B.C

During the middle ages (AD 450- 1450) there was a steady
2nd stage development in the use of lubricants, but it was not until AD 1600 –
1850.

In1859, Colonel William introduced the petroleum industry. He

3rd stage drilled first oil well at Titusville, Pa in America.

In 1950, multigrade oils were first introduced which improved the

4th stage hot and cold performance of the oil.

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 Lubricants

What is Refining (also called affining) is the process

of purification of a substance.
refining
A chemical engineering process used to
Oil refining transform crude oil into useful products.

Oil refining
products

Kerosene
Jet fuel
Diesel oil
Petrol

5
Functions of Lubricants

Absorb and transfer heat

Protect surfaces from corrosion

Separate moving surfaces

Transport contaminants to filters

Transmits force and motion

6
 Moving Surfaces – Lubrication –
Particle Generation
LOW LOAD VERY HIGH LOAD

High Speed
Very Low Speed

Hydrodynamic Boundary
Lubrication Lubrication
 Laminar Flow  Boundary Films
 Film thickness several  Viscous oil properties
times greater than surface ineffective
roughness
 Formation of Lubricants

Lubricants are prepared with the combination of:

Base Stock Additives

Oil from Different

Refinery Chemicals

70% 30%

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 Additives
What they are
Organic and inorganic compounds dissolved or suspended in oil Can
represent from 0.1% to 30% of formulated oil volume Monitoring
additive health is an important goal of oil analysis.
Machine Common additives used Percent of
oil volume
Important
Engines Anti oxidant,corrosion 10-30 %
Additives inhibitor,dteregent,anti wear,anti foam
Antioxidant
Steam turbines Anti oxidant,corrosion ,anti faom,anti 0.5-5%
Dispersants and emulsifies
compressors
Corrosion Inhibitor Gears Anti oxidant,anti wear.anti foam, 1-10%
Extreme pressure,sometime corrosion
VI Improvers inhibitor

Anti foam agents Hydraulic Anti oxidant,Anti wear,Anti 2-10%

systems faom,corrosion inhibitor,pour point
depressent,viscosity index improvers

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 Additives
An antioxidant is a molecule that inhibits the oxidation of
Antioxida other molecules.
nt

To prevent the formulation of acids, varnish,

Function sludge and high viscosity that normally results
from oxidation

Antioxidants decompose reactive hydro peroxides

Working
and free radicals before they lead to oxidation

Aromatic amines, Zinc Dialkyl dithiophosphate

Common (ZDDP)
types

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 Additives
An additive which is used to disperse sludge and soot
Dispersan particles for the purpose of preventing agglomeration,
ts settling and deposits.

Head: Polar – Water Based

Dispersants envelopes particles and keep them

firmly divided in an homogenies manner.

It does not allow the particles to get

concentrated at one location

Tail: Non-polar – Oil Based

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 Additives
Corrosion inhibitor forms a polar adherent film
Corrosion to steel and cast iron surfaces to repel water
Inhibitor which inhibits rust formation.

Corrosion inhibitor
range
Phosphoric acid esters
Fatty acid amides
Carboxylic acid derivatives
Boric acid amine blends
Alkanol amides

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 Additives
Viscosity Index is an arbitrary measure for the
Viscosity change of viscosity with temperature.
Index
VI Improvers tries to minimize the effects of
VI Improvers varying temperature on lubricants

It is used to characterize lubricating oil in the

Use:
automotive industry.

Vi
improver
Ethylene propylene copolymers
s
Polyisobutylene

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 Additives
An anti-foaming agent is an additive that reduces the
Anti-Foam formation of foam (air bubbles) in industrial process
Agents liquids

Functions

Anti foam use silicone to weaken surface

bubbles allowing them to quickly collapse.

They expands the air bubbles and move them

to the surface to explode.

Compounds used includes methyl silicones

and organic polymers. Blended into base oil
at 5-10ppm.

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Monitoring Oil

Baseline new oil

Continue Using
Routine analysis

NO

YES

CORRECT CAUSE OR
CHANGE OIL
 Oil/lube Analysis
Oil
analysis

Oil analysis (OA) is the laboratory analysis

of a lubricant's properties, suspended
contaminants, and wear debris.

OA is performed during routine preventive

& predictive maintenance to provide
meaningful and accurate information on
lubricant and machine condition.

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 OIL ANALYSIS CAN TELL YOU
Monitor changes in lubricant properties
Lubricant determined suitability for continued use.
health
Silicon Viscosity, Total acid number,
Additive Total Base number
information
Equipment Gives overview of asset’ health
health
Iron, Cr, Ni, Cu, Pb, Sn, Cd, Silver,
Detect wear Vanadium
metals

 Water
CONTAMINANTS  Fuel Dilution
 Soot
 Tribology
What is Interacting surfaces in relative motion.
Tribology
Tribology refers to the study of friction, wear, lubrication and contact
mechanics, particularly in and engineering and mechanical context.

Surface

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 Elements of Tribology
Mechanical wear is the
undesirable removal of material
from a surface.

Wear

Contamination Chemistry

Chemistry changes include Contamination is any substance

lubricant degradation and additive foreign to the lubrication system
depletion. which is not dissolved by the oil.

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Typical Problems Detectable By Oil
Analysis

Early signs of abnormal wear

Failure of gaskets

Blockage of oil filters

Inefficient air filters

Incorrect injector timing

Condition of the lubricant

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 Benefits of oil analysis

Lubricant consolidation

Extended oil change intervals

Extended machine life

Make money and save money

Preliminary Inspection of an Oil Sample
Initial oil tests are based on Visual Inspection

 Presence of free water

 Presence of gross shining metal particles
 Color of the oil
 Sedimentation of insoluble material
 Fuel dilution and odor
Three categories of oil analysis
FLUID PROPERTIES
ANALYSIS
 Oil Properties
Oil properties
Density Viscosity

Acid number Oil Base number

Elemental analysis Water

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 Oil Properties
The viscosity of a fluid is a measure of
Viscosit its resistance to gradual deformation by shear
y stress or tensile stress.

Types of
viscosity
Absolute Viscosity

Kinematic Viscosity

Intermolecular Forces

Intermolecular &
Gravitational Forces
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 Oil Properties

Kinematics viscosity
measurement.
 Oil is drawn into the tube by suction.

 Tube is submerged in constant

temperature bath.

 Time is measured in
seconds as fluid flows from start to
stop mark.

 Kinematic Viscosity = apparatus

constant x efflux time.

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 Oil Properties
Viscosity limits

Severe
Limit Crankcase Oils** Industrial Oils** Environment
Industrial Oils**

Critical (upper) +20% +10% +7%

Critical (lower) -10% -10%* -10%*

*Twice this amount for oils with VI improvers.

**Crankcase oil limits based on cSt @ 100°C, industrial oils based on cSt @ 40°C.

Note: Severe environment oils are at high risk for thermal and oxidative degradation.

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 Oil Properties
Total acid number
The total acid number (TAN) is a measurement of acidity that is determined
by the amount of potassium hydroxide in milligrams that is needed to
neutralize the acids in one gram of oil.

Function
s:
 Trends depletion of certain additives
 Identifies the onset of base stock oxidation
 Measure the level of corrosive acids
 Measure the level of reserve alkalinity

TAN increase results in additive depletion – Rule of Thumb: TAN < 1

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 Oil Properties
Total base
number:
Total base number (TBN) is a measure of a lubricant's reserve alkalinity.
It is measured in milligrams of potassium hydroxide per gram (mg
KOH/g).

Function
s:
 Trends depletion of certain additives
 Identifies the onset of base stock oxidation
 Measure the level of corrosive acids
 Measure the level of reserve alkalinity

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 Oil Properties
Basic number standards
 ASTM D2896 and ASTM D4739 both use potentiometric
titration as their fundamental tool to measure BN.

 ASTM D974 and ASTM D5984 are methods that use color-
indicator titration to determine the basic constituents in
petroleum products and lubricants.

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 Viscosity index ASTM-D2270
Parameters
 An oil change in viscosity with respect to change in temperature is
represented by its viscosity index.

 The larger the viscosity index the smaller the change in viscosity with
temperature.

 The viscosity index of an oil can be calculated by determining

experimentally its viscosity at 40 degree C and 100 degree C.

Viscosity -20 to 0 0 to 60 60 to 100 to 200

Index 100
Typical oil Some Naphthenic Paraffinic VI improved mineral oils and synthetic,
phosphate mineral oil mineral e.g diasters polyolesters polyglycols.
esters oil

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 Rotating pressure vessel oxidation test

(PRVOT)
Tests the oxidation stability of used oil
 Results are reported minutes(of oil life)
 Mainly used for Turbine Oil Monitoring
 Color (ASTMD1500)

Color test
Test is used for manufacturing control purposes. It is important
since color is readily observed by customer.

Equipmen Colorimeter
t
Benefits
No direct significance in quality.

Ensure product uniformity.

Appreciable change from normal

indicates contamination.
 Copper strip corrosion
(ASTMD130)
Qualitative measure

This test indicates presence of corrosive

sulphur in petroleum products

A qualitative measure of the tendency of a

petroleum product to corrode pure copper.

Causes
Improper refining

Improper storage condition

 Foaming tendency (ASTM
D892)
Function
Foam tendency describes the amount of foam generated immediately
after the fluid is aerated, the foam stability quantifies the amount of foam
remaining 10 minutes after stopping of aeration

Control Additives Used to Control Foaming Tendency.

 Elemental Spectrometry

Quantifies the amount of inorganic elements in

Functi
the oil.
on
AES
Rot Rode Spectroscopy,
Method
ICP
s Atomic Absorption (AA)

Reporti
ng
Results are reported in parts per million (ppm).
Elements are categorized as wear, additives, and contaminants.
Some particle size limitations - less than 8 microns (depending on the
instrument used, the limitation may be much less.)
CONTAMINATION ANALYSIS
 Water Test

Water is the second most destructive

contaminant.

It can

 Change oil viscosity.

 Rust and corrosion
 Change Acidity
 Make Sludge & Sediment
 Water
contaminated oil
Dissolved Water

Water particles are too

small and attached to
the oil molecules.

Free Water

It settles down in a
separate region

Emulsified Water

This results in
suspended water
particles and give hazy
appearance
 Water tests
Crackle Test No visible or audible change.

 Used to screen samples for

water contamination. No free or emulsified water

Very Small Bubbles (0.5 mm) produced and quickly disappear.

 A hotplate is heated to ~ 300
f, a small amount of oil is
placed on the heated surface 0.05 - 0.1% 500-1000 ppm

for this test.

Bubbles approximately 2 mm are produced, gather to center, enlarge to 4mm, and disappear quickly.

0.1 - 0.2% 1000-2000 ppm

Bubbles 2-3 mm are produced growing to 4 mm, process repeats, possible violent bubbling and audible
crackling.

0.2 and more >2000 ppm

 Water tests

Karl Fischer Titration

 Titration method using reagents (Iodine) which react with the

water.

 Quantifies the amount of total water, reported in ppm or %age

 Lower detection to 30 ppm

 Water, what is ok?

Acceptable levels:
 Typically below 250 PPM.

 You can see water at around 900 PPM.

Water removal
methods
 Life extension table-
moisture
Life Extension Factor

ppm 2 3 4 5 6 7 8 9 10

50,000 12,500 6,500 4,500 3,125 2,500 2,000 1,500 1,000 782

25,000 6,250 3,250 2,250 1,563 1,250 1,000 750 500 391

10,000 2,500 1,300 900 625 500 400 300 200 156

5,000 1,250 650 450 313 250 200 150 100 78

Current Moisture Level
2,500 625 325 225 156 125 100 75 50 39

1,000 250 130 90 63 50 40 30 20 16

500 125 65 45 31 25 20 15 10 8

250 63 33 23 16 13 10 8 5 4

100 25 13 9 6 5 4 3 2 2

Table of Moisture Life Extension Method

 Ash content
(ASTMD874)

Metallic
deposits
Metallic deposits formed in the
combustion chamber & other engine parts
during the high temperature operation.

They can
affects
 Fuel injection systems.

 Induces boiler corrosion.

 Attacks refractory lining.

 Flash point tests(ASTM
D92)
Measuring Ambient to 400 degree C
range
Important indication
Flash point controls flammability property
of petroleum products

In used crankcase oils, lower flash

indicates fuel dilution

Indicates degree of safety in storage,

transportation and use

Flash point test gives an indication of

presence of volatile components in an oil
 Particle counting test

 Ability to specify target cleanliness levels for Systems, machines, and

incoming lubes.

 Ability to implement Contamination Control.

 Used to determine filtration specifications and efficiencies.

 Trending allows early indication of abnormal wear and increases in

contaminant levels due to outside influences.
 Three ways to count and
size particles

 Using a Microscope (ISO 4407)

 Optical Particle Counting(ISO 11500)

 Automatic Pore Blockage particle counting (BS 3406)

 Optical particle
counters

Light blockage particle counter Light scattering particle counter

Pore blockage particle
counter
 ISO particle
counts
It is important to understand what ISO Particle Counts are
What is it?

Quantitative analysis
Quantitative analysis of oil is used to determine the distribution of
particle sizes in the oil.

Why ?
Try to keep oil at a cleanliness level to prevent wear and failures.

Targeted to remove clearance size particles out of the oil.

 ISO
Code range
 NAS 1638

NAS 1638 Class Number, of Particles per 100ml in

5 to 15 15 to 25 25 to 50 50 to 100 > 100
00 125 22 4 1 0
0 250 44 8 2 0
1 500 88 16 3 1
2 1000 178 32 6 1
3 2000 356 63 11 2
4 4000 712 126 22 4
5 8000 1425 253 45 8
6 16000 2800 506 90 16
7 32000 5700 1012 180 32
8 64000 11400 2000 360 64
9 128000 22800 4100 720 128
10 256000 45600 8100 1440 256
11 512000 91200 16200 2800 511
12 1000000 182000 32400 5800 1024
13 2048000 364800 64800 11520 2048
14 4096000 729600 129600 23040 4096
15 8192000 1459200 259200 46080 8192
16 16384000 2918400 518400 92160 16384
17 32768000 5836800 1036800 184320 32768
18 65536000 11673600 2073600 368640 65536
 Particle counting benefits

 Verifies filter performance

 Verifies pump condition
 Verifies stored lubricant cleanliness
 Identifies changing atmospheric contamination
 Confirms systems flushing
 Identifies the need for ferrographic analysis
 Determines optimum filter change point
 Identifies new filter defects
 Verifies centrifuge performance
 Particle counting benefits

 Detects high corrosive wear

 Verifies bearing condition

 Confirms target cleanliness levels are achieved
 Oil quality n Identifies abnormal gear wear

 Identifies use of dirty top-up containers

 Verifies shaft seal exclusion performance
 Determines new oil cleanliness

 Identifies oil film failure problems

WAER DEBRIS ANALYSIS
 Wear debris analysis

Wear debris analysis (WDA) is an attempt to

WDA determine the condition of machinery through
the examination of the particles generated by
wear process.
 Wear debris
analysis
Procedure steps

Obtain an oil sample from a machine.

The sample is then diluted with a solvent.

Draw the sample through a membrane filter or use a

magnetic separation technique such as the rotary particle
depositor to separate the solids from the fluid.

In the laboratory take a measured amount of the fluid and

deposit into a clean beaker.
 Wear debris
analysis
Procedure steps
Wear debris analysis is a relatively simple procedure not requiring a
high skills level to perform.

Repeat the procedure at a decided time interval.

Even so the results give a direct indication as to the level of threat

and damage within industrial drives absent from some of the more
sophisticated techniques.
 Wear debris
analysis
The amount of ferrous wear is quantified by means of a debris analyzer such
as the PQ2000 manufactured by Swansea Tribology Centre.
Visually analyze the debris at 100x magnification under a reflected light

Parameters
 Type of particle
 Mechanism of removal
 Average particles size
 Maximum particle size
 Contamination index

Health status is a parameter between 1 -5 with 1 being a healthy machine

and 5 being a machine which is imminently threatened with failure.
 Purpose of Oil Analysis Tests by
Machine Applications
Diesel Engine Gear System Hydraulic System

wear, contaminants, additives gear boxes generate all sorts of will often validate or clarify particle
Elemental Viscosity – contamination wear, but the levels can count; added value for additives and
from soot, or fuel sometimes get confusing contamination
Particle quantitative, somewhat holistic
Count
tracks the large iron-laden
Ferrography particles for Analytical
Ferrography trigger
oxidation, nitration oxidation, base stock integrity oxidation, base stock integrity
FTIR combustion byproducts
contamination from soot, or always useful and worthwhile always useful and worthwhile
Viscosity fuel
TAN contamination or degradation contamination/degradation

TBN reserve alkalinity, detergency

mostly to identify an invalid to validate the sample any detectable amount is probably
Water sample abnormal or critical + need particle
count validity check
excessive idling or
mechanical issue, such as a
Fuel Dilution nozzle dribbling or leaking
injector seal
combustion cycle indicator,
Fuel Soot Air fuel ratio
 Frequency of Oil Analysis Tests by
Machine Applications
Large Large
Air/Gas Diesel Hydraulic Gear Rolling Industrial
Test Compressor Engine System Boxes Element Turbines
Bearings
Spectroscopy R R E R* R* R

FT-IR R R X X X X

Viscosity R R R R R R

Analytical E E E E E E
Ferrography
TAN R X R R R R

TBN X R X X X X

Particle Count R E R E E R

Moisture R R R R R R

R = Test is routine.
E = Test is performed on exception when triggered by an out of limit test.
* = Rotrode Filter Spectroscopy (RFS) should be used to detect and quantify large particles.
X = Test is not performed.
 Storage of lubricant

 Indoor Storage

– Indoors in a ventilated room.

– On racks off the floor.
– On their sides, not upright.

 Outdoors storage (even temporarily)

– On their sides undercover with

openings positioned at 3 and 9 o’clock
– Shelter them to protect from rain,
snow and other elements
 Handling of containers

Important checks

 Drums should be rolled rather than dragged.

 Make sure all transfers take place under clean

conditions to avoid contamination.

 Containers are kept tightly closed when not in use.

 Dispensing of lubricants
Important checks

 Use the oldest lubricant first.

 Test the lubricant before use, if in doubt.
 Different lubes should never be mixed in dispensing containers or
transfer equipment.
 Containers should be clearly marked.
 Always check if the dispensing equipment is clean.
 Keep the dispensing containers tightly closed when not in use.
 Avoid open-topped containers.
 No smoking around lubricant and solvents.
 OIL SAMPLING THE VERY
BEST
PRACTICES
 Oil sampling objectives

Three Objectives to Good sampling

 Maximize Data density

 Minimize data disturbance

 Proper frequency
 Sampling hints
Useful hints
Mark the sample bottle prior to actually taking the sample

Never re-use sampling tube, discard after one use

As soon as the sample is taken, replace the cap.

Do not take the cap off the sample bottle until you are ready to sample

Do not take the cap off the sample bottle until you are ready to sample

This will help to keep dust, moisture, and dirt out of the sample

Over time, some contaminants will agglomerate and cling to the bottle walls
 Sampling hints
Useful hints
Tests should be conducted within a reasonable time frame.

The best samples are obtained after a machine is shutdown.

When drawing oil through a drain plug or valve,

do not collect oil during the initial spurt or rush.
 Sampling frequencies

 Begin by sampling on a monthly basis to quickly establish trends and

identify immediate problems.

 Different machines have different intervals.

 Continue monthly sampling for the first 3 to 6 months.

 Modify sampling intervals based on the historical data collected and/or

the criticality of the machine
 Oil sampling interval
Fluid Type or System Regular Use Intermittent Use
Gear Drives 500 hours or monthly quarterly
Compressor 500 hours quarterly
Turbines 500 hours quarterly
Hydraulic Systems 500 hours or monthly quarterly
Diesel Engines 500 hours quarterly
Natural Gas Engines 500 hours quarterly
Transformers quarterly annually
Hot Oil Systems 500 hours quarterly
HVAC Compressors 250 hours quarterly
HVAC Refrigerants quarterly annually
Coolants 500 hours quarterly
Vehicle Fuel Tanks as needed as needed
every shipment of new product every shipment of new product
New Diesel Loads
or supplier or supplier
Diesel Storage Tanks quarterly quarterly
 Clean oil sampling procedure

 In clean air environment place capped bottle into a

clean zip lock bag and seal

 Place individual bags into large zip lock bag, include

sampling device

 Just prior to sampling ,remove bottle cap without

opening

 Thread bottle onto probe on or vacuum sampling

device, without opening bag

 After sampling place cap tightly onto bottle without

opening

 Remove bottle from bag, label bottle and dispose of

bag
 Sampling bottles
An important factor in obtaining a
Important representative sample is to make sure
the sampling hardware is completely
factor flushed prior to obtaining the sample

An appropriate bottle needs to be selected

for the application and the test that is
Appropriate bottle planned. Several features including size,
material and cleanliness must be considered
when selecting a sample bottle.

Another consideration in selecting the

bottle size is that the entire volume of the
Entire volume
bottle should not be filled with fluid during
the sampling process.
 Guide lines for filling bottles

Low viscosity (ISO VG 32 or less) - Fill to about three-

fourths of the total volume.

Medium (ISO VG 32 to ISO VG 100) - Fill to about

two-thirds of the total volume.
viscosity
(over ISO VG 100) - Fill to about one-half of
High the total volume
viscosity

75