Tribology

What is tribology? Oil analysis involves sampling and analyzing oil for various properties and
materials that indicate wear and contamination in an engine, transmission or hydraulic system.
Sampling and analyzing on a regular basis establishes a baseline of normal wear and can
indicate when abnormal wear or contamination occurs.
An oil analysis tells you a lot about how the equipment was used and what condition it's in. Oil
that has been inside any moving mechanical apparatus for some time reflects the exact condition
of that assembly. As moving parts make contact, wear occurs and introduces minute metal
particles to the oil. These particles are so small that they remain in suspension. Many products of
the combustion process also become trapped in the circulating oil. In addition, the oil may be
exposed to external contamination. Identifying and measuring these impurities indicates the rate
of wear and level of contamination. Thus, the oil becomes a working history of the machine. An oil
analysis also suggests methods to reduce accelerated wear and contamination.
A typical oil analysis can indicate the presence of contaminants and tell you if you've been using
the appropriate lubricants. Oil analysis detects:
Fuel dilution of lubrication oil
Dirt contamination in the oil
Antifreeze in the oil
Excessive bearing wear*
Misapplication of lubricants.
Some wear is normal. However, abnormal levels of a particular material can give an early warning
of impending problems, prevent a breakdown and allow for corrective action such as repairing an
air-intake leak before major damage occurs. One major advantage of an oil-analysis program is
being able to anticipate problems and schedule repair work to avoid downtime during a critical
time of use. Early detection can:
Reduce repair bills
Reduce catastrophic failures
Increase machinery life
Reduce non-scheduled downtime.

Evaluating used equipment.

A complete record of oil analyses you've performed can prove to be a great tool when selling a
piece of used equipment. It shows the potential buyers how you have maintained the equipment
as well as any adjustments you made to it during its life. The history also is a good indicator of
potential future repairs and overhaul requirements. When buying a piece of used equipment
yourself, you also can take advantage of the benefits an oil analysis can offer. However, without
knowing the amount of operation of the oil being analyzed, you should consider the test
conclusive only if it indicates a problem. A good report could result from either no problems or a
short length of service of the oil.

Taking an oil sample

It is important to take an oil sample that is representative of all the oil in the machine and that
there is no chance of contamination from dirty bottles or dirt entering from the sample cock..
Always be sure the oil is hot and thoroughly mixed before sampling. Handle hot drained oil with
care as it could cause serious burns. The easiest time to obtain a sample may be when the oil is
being drained for an oil change. Sampling at this time usually involves letting some of the oil drain

and then catching a sample in an appropriate container. You also can obtain samples without
draining oil by suctioning oil out through plastic tubing routed down into the oil reservoir. In any
case, it is important to have an appropriate container and follow sampling directions thoroughly. A
lot of testing laboratories will provide you with a kit that includes a sample bottle. Many of the
tests are for measuring materials on a parts-per-million basis. So, the container must be sterile or
the test may pick up contaminants what was in the container before.

Cost and convenience

Cost of oil analysis will vary according to the laboratory and extent of the analysis. Typical
charges are $10 to $30 per analysis. You can justify the expense of the analysis if it alerts you to
a major problem that you can correct in the off-season and prevents downtime when you need
the machine. Several companies have developed oil-analysis kits that make oil analysis
convenient. These kits include the sample bottles, suction pump and tubing, and sometimes a
pre-addressed, postage-paid mailing container.

Results
Typically, you will receive the results of the laboratory analysis 2 to 4 days after the lab receives
the sample. The laboratory may note when the analysis shows an abnormal condition and issue a
caution or recommendation accordingly. Typical recommendations might be:

Example 1: Bearing metals indicate wear. Inspect all bearing areas for wear. Resample at
half interval.
Example 2: Unit is in satisfactory condition. Resample at normal interval.
Example 3: Abrasion indicated. Inspect air-filtration system. Upper cylinder wear
indicated. Excessive fuel dilution. Resample at half interval.

Optimum maintenance interval

Most maintenance experts realize that the "average need" usually determines the oil-change
intervals for both engines and transmissions. No two pieces of equipment have the same
preventive maintenance needs. Each machine has different imperfections and operates under
different conditions. Operators performing smaller or lighter jobs can cause different conditions on
engine and transmission wear than those that occur during more extended use. When using oil
analysis to determine maintenance intervals, little guesswork exists. Records show that some
equipment can run safely two or three times longer than recommended intervals. The oil analysis
may show that you are changing the oil more often than necessary-or not often enough.
By eliminating too-frequent oil changes, you reduce the cost for oil and servicing, and also reduce
the amount of used oil with which you must deal. This is an important pollution-prevention
method-reducing the source.

Which Measurement Parameters?

Because of the root cause focus of proactive maintenance, the areas of interest in an on-site CM
strategy may include:

Solid Particle Counts

Associated with the root cause of system wear and additive depletion.

ISO Cleanliness
Particularly useful on hydraulic circuits where cleanliness is paramount

Viscosity
Associated with determining either fluid dilution, incorrect lubricant or as an indicator of
the lubricants remaining useful life.

Moisture
Preferably maintained below the saturation point to avoid additive scrubbing and system
corrosion.

Total Acid Number (TAN) or Total Base Number (TBN)

Associated with the remaining useful life of the lubricant.

Analytical Ferrography
Intensive method for determining the how and why of ferrous contamination.
Parameters that are often logged but not correlated in a CMMS system may include process or
consumption variables:
Lubricant Make-Up or Consumption - unacceptable levels are usually associated with
a poor lubricant strategy in terms of handling and contamination control.
Filter Life and Rate of Blockage - when specified correctly, filters should, in most
applications, have at least a six-month life, and sudden change in the rate of filter
blockage may indicate a system fault.
System Operating Variables Such as Temperature, Pressure, Power Demand,
Emissions, etc. - changes in these values may indicate deterioration in performance that
could adversely impact productivity and quality.

Solid Particle Counts

Figure 1 Particle count technique - v - particle size

Spectrometric Analysis:
Technique for detecting and quantifying metallic elements in a used oil resulting from wear,
contamination and additives. The oil sample is energized to make each element emit or absorb a
quantifiable amount of energy, which indicates the elements concentration in the oil. The results
reflect the concentration of all dissolved metals (from additive packages) and particulates. This
test is the backbone for all oil analysis laboratories today, as it provides information on machine,
contamination and wear condition relatively quickly and accurately.
Its major limitation is that its particle detection efficiency is poor for particles 5 microns (m) in
size or greater. Particles greater than 10 m in major diameter are the result of abnormal; wear
modes, and these particles must be quantified. The technique is accurate to 10%, although new
equipment is now reporting within 3%.

Rotrode Filter Spectroscopy:

First introduced in 1992, this spectrometric technique detects and large or coarse wear metals
and contaminants in a used oil sample. "Coarse" particles include all particulates up to 25 m in
size but excludes all additives. "Coarse" particles are especially important since these particles
are the first indicators of abnormal wear situations. It is superior to DR(direct read)ferrography
because it detects ferrous, nonferrous and contaminant elements (usually 12 elements).
Detection efficiency of large material gets poorer as particle size increase above 25 m diameter.
Its accuracy range is within 15%.

ISO Cleanliness Particle Count

How the ISO 4406 Cleanliness Standards Work
The smallest item that can be seen by the naked eye is 80 microns, which is about the diameter
of a human hair. Oils normally contain many thousands of particles smaller than the eye can see.
The purpose of the ISO 4406 Cleanliness Standards is to provide a universal reporting method
for the particle contamination of fluids. This is done by counting the particles in a 1 millilitre
sample of the fluid, which is roughly equal to one eyedropper of fluid.

Table 1 ISO 4406 Chart

1st All particles equal to or greater than 2 microns are counted.

2nd All particles equal to or greater than 5 microns are counted.
3rd All particles equal to or greater than 15 microns are counted.
Using the ISO 4406 Chart above, the fluid is given a cleanliness rating based on how many
particles of each sampling were counted.

Figure 2 ISO 21/19/17 fluid (magnification 100x)

Figure 3 ISO 16/14/11 fluid (magnification 100x)

ISO 4406 Example

For example, a 1 millilitre sample of fluid containing:
2200 particles >/= 2 microns
450 particles >/= 5 microns
60 particles >/= 15 microns
Would have an ISO Cleanliness Level of 18/16/13 as shown in the graphic below.

Viscosity
Contrary to popular opinion, oil does not "wear out" at some specific point, and be 100% OK
before that point. It is a gradual process that begins as soon as new oil is first cycled through a
running engine. The oil does hold up better when new, and starts deteriorating faster as it has
been used more, though. So there is no magic point when you should change your oil, where it is
a waste of money to do so before that point, and very, very bad for the engine past some other
specific mileage.
"Wear" on oil consists of things like breakage of the molecular chains, viscosity deterioration,
dilution with contaminants, and breakdown or depletion of various additives. These are all gradual
processes. And, yes, modern oils are much, much, better than older oils and can be used longer.
(However, some of the problems, such as dilution, happen just as quickly as they used to).

Dynamic viscosity
The dynamic viscosity is the viscosity that relates shear stress and shear rate du/dz in a fluid,
i.e. = du/dz. The viscous shear stress is proportional to the shear rate, the dynamic viscosity

being the proportianality factor. So, thicker oils have a higher viscosity value causing relatively
higher shear stesses at the same shear rate.
Dynamic viscosities are usually measured under high shear conditions, for example, the cylinder
viscometer in which the viscous shear torque is measured between two cylinders.

Kinematic viscosity
The kinematic viscosity is the quotient of the dynamic viscosity and the fluid density , =/.
The physical principle of measurement is based on the rate at which a fluid flows vertically
downwards under gravity through a small-diameter tube.

SI Viscosity classificaton
ISO 3448, where ISO VG 22 refers to a viscosity grade of 22 cSt 10% at 40C.
SAE Viscosity Grades for Engine Oilsa SAE J300 Dec 99
The actual viscosity grade of a lubricant is determined by the Society of Automotive
Engineers, for example SAE-15W40 for a multigrade oil and SAE-40 for a monograde oil.
The first number (15W) refers to the viscosity grade at low temperatures (W from winter),
whereas the second number (40) refers to the viscosity grade at high temperature.
Table 2 Oil viscosity guide

SAE
Viscosity
Grade

0W
5W
10W
15W
20W
25W
20
30
40
40
50
60

Low Temperature Viscosities

High-Temperature
Viscosities

Crankingb
Pumpingc
Kinematicd
(mPa.s)
(mPa.s)
(mm2/s)
max at tempmax at temp
at 100C
C
C
min max
6200 at -35 60 000 at -40 3.8
6600 at -30 60 000 at -35 3.8
7000 at -25 60 000 at -30 4.1
7000 at -20 60 000 at -25 5.6
9500 at -15 60 000 at -20 5.6
13 000 at -10 60 000 at -15 9.3

5.6 <9.3

9.3 <12.5

12.5 <16.3

12.5 <16.3

16.3 <21.9

21.9 <26.1

High
Sheare
Rate
(mPa.s)
at 150C
min

2.6
2.9
2.9
3.7
3.7
3.7

Moisture (Water) Content

Water is perhaps the most harmful of all contaminants with the
exception of solid particles. While the presence of water is
often overlooked as the primary root cause of machine
problems, excess moisture contamination can lead to
premature oil degradation, increased corrosion and increased
wear.

Visual Crackle Test

The simplest way to determine the presence of water in oil is to
use the Visual Crackle test. While this is an effective test for
identifying free and emulsified water down to say 500 ppm, its
biggest limitation is that the test is nonquantitative and fairly
subjective. False positives are possible with entrained volatile
solvents and gases. Nevertheless, as a screening tool in the
lab and the field, the crackle test will always have a role to play
where a quick yes or no answer is required for free and
emulsified water.

FTIR Analysis
FTIR can be an effective method for screening samples
containing in excess of 1,000 ppm of water, provided a correct
new oil baseline is available for spectral subtraction. However,
due to its limited precision and comparatively high detection
limits, FTIR is not adequate in many situations where precise
water concentrations below 1,000 ppm or 0.1 percent are
required.

Dean and Stark Method

The classic method for determining water-in-oil is the Dean
and Stark distillation method (ASTM D95). This test method is
fairly cumbersome and requires a comparatively large sample
to ensure accuracy, which is why it is rarely used in productionstyle oil analysis labs today. The method involves the direct
codistillation of the oil sample. As the oil is heated, any water
Figure 4 Dean and Stark
present vaporizes. The water vapors are then condensed and
Distillation Apparatus
collected in a graduated collection tube, such that the volume
of water produced by distillation can be measured as a function of the total volume of oil used.

Karl Fischer Moisture

The Karl Fischer Moisture test is the method of choice when accuracy and precision are required
in determining the amount of free, dissolved and emulsified water in an oil sample. However,
even within the scope of Karl Fischer testing, there are several methodologies that are used.
All Karl Fischer procedures work in essentially the same way. The oil sample is titrated with a
standard Karl Fischer reagent until an end-point is reached. The difference in test methods is

based on the amount of sample used for the test and the method used to determine the titration
end-point.
The most frequently used Karl Fischer method follows ASTM D1744 and involves volumetric
titration of the sample, using a potentiometric cell to determine the end-point. While this method is
reliable and precise, there can be reproducibility problems at low water concentrations (200 ppm
or less). In addition, the test can be subject to interferences from sulfurous additives (for instance,
AW and EP-type additives) and ferric salts which may be present due to wear debris. Both of
these react with the Karl Fischer reagent as if they were water and can give a false positive,
resulting in an overstating of the water concentration. In fact, a new, clean, dry AW or EP oil may
give a reading of as much as 200 to 300 ppm, due to the reaction of the additives, rather than
because of excess moisture.
More recently, labs have been switching to a coulometric titration method described in ASTM
D6304. This method is more reliable than D1744 at low water concentrations and is less prone to
interference effects, although again, AW and EP additized oils can show as much as 100 ppm of
water as a result of the effects of the sulfurous additives.
The most reliable method is ASTM D6304, complete with codistillation. With the codistillation
method, the oil sample is heated under a vacuum so that any water present in the sample
evaporates. The water vapors are condensed and dissolved into toluene, which is then titrated
using the D6304 procedure. Because the additives and other interfering contaminants that may
be present in a used oil sample remain dissolved or suspended in the oil, the condensed water in
the toluene is free from interference effects and is a true count of water present in the sample.
Another less commonly used method is ASTM D1533, which is used for determining water
concentrations down to 10 ppm or less in transformer oils using a coulometric Karl Fischer
reagent.

Calcium Hydride Test Kits

One of the simplest and most convenient ways to determine water concentrations in the field is by
using a calcium hydride test kit. This method employs the known reaction of water with solid
calcium hydride to produce hydrogen gas. Because the reaction occurs stoiciometrically, the
amount of hydrogen gas liberated is directly proportional to the amount of water present in the
sample. Therefore, the water content of the sample can be determined by measuring the rise in
pressure in a sealed container due to the liberation of hydrogen gas as any water in the sample
reacts with the calcium hydride. Used correctly, these test kits are reported to be accurate down
to 50 ppm free or emulsified water.

Saturation Meters
When the amount of water present in an oil sample is below the saturation point, saturation (dewpoint) meters can be used to indirectly quantify water content. The saturation point of an oil is
simply the point at which the oil contains as much water in the dissolved state as possible, at a
given temperature. At this point, the oil is saturated or has a relative humidity of 100 percent. ...
Most saturation meters use a thin film capacitive device, whose capacitance changes depending
on the relative humidity of the fluid in which it is submerged. Saturation meters have proven to be
accurate and reliable at determining the percent saturation of used oils.
The biggest drawback with saturation meters is the fact that the saturation point is strongly
dependent on temperature as well as the presence (or absence) of polar species, including

additives, contaminants and wear particles. In addition, with water levels in excess of the
saturation point, typically 200 to 600 ppm for most industrial oils, saturation meters are unable to
quantify water content accurately. Despite these limitations, saturation meters can be a useful
trending tool to determine moisture onsite, provided they are used frequently and routinely.
Monitoring and controlling water levels in any lubricating system is important. Whether it is a large
diesel engine, a steam turbine, a hydraulic system or an electrical transformer, water can have a
significant impact on equipment reliability and longevity. Regular water monitoring, whether it be a
simple onsite crackle test or a lab-based Karl Fischer moisture test should become a standard
condition-monitoring tool. But remember, like all tests, the methods used to detect water in oil
have strengths and weakness, so be sure to select the one that meets your needs and desired
detection limits.

TAN and TBN

TAN
Total Acid Number, or TAN, is the measure of both the weak organic and strong inorganic acids
present in oil. It is applicable to gearbox, gas engine, gas turbine, synthetic and hydraulic lubes.
TAN is not generally associated with engine crankcase lubricants, unless they are severely
contaminated. The singular exception to this may be crankcase lubricants for gas engines. In this
instance, TBN can deplete very rapidly and elevated operating temperatures can generate high
levels of weak organic acids
A rise in TAN is generally associated with oil oxidation due to time and /or operating temperature.
Trend as well as absolute values should be used to monitor TAN.
High combustion temperatures in gas engines (especially ones using a stoichiometric (1:1)
Air/Fuel ratio) will lead to rapid TBN depletion. This is further exaggerated when using landfill gas
where typical oil life is less than 500 hours. Under these circumstances, high TAN and viscosity
usually become the limiting parameters for oil life.
High TAN will cause:

The formation of gums and lacquers on metal surfaces.

(Associated with) increased viscosity of pumping losses.

A gradual speed up in the rate of TAN increase.

System corrosion, particularly if water is present.

Determining the concentration of strong acids:

Titration with a strong base (specifically KOH) will begin at a pH of less than 4.2 and
produce a Strong Acid Number (SAN) at an end point of about pH 4.2.
Determining the concentration of weak acids:
Titration with a strong base will begin at a pH above 4.2 and produce an Acid Number at
an end point of about pH 11.
In the case of the strong acid titration we add only enough base (OH -) to shift the equilibrium up
to pH 4.2. In the case of a weak acid titration we add just enough base to shift the equilibrium
from some point above 4.2 to a pH of about 11.

Total Acid Numbers (TAN):It follows then, that if both strong and weak acids are present, the Acid
Number (commonly referred to as Total Acid Number, TAN) for the system is obtained by titrating
to pH 11. The amounts of each type of acid can be obtained by noting the amount of KOH used to
reach pH 4.2 for the strong acids and the incremental amount of KOH added between pH 4.2 a
pH 11 for the weak acids. These may be recorded as Strong Acid Number and Weak Acid
Number respectively with the TAN being the sum of the two.

TBN
It is important to understand that all test methods are subject to some normal, predetermined
variability, depending on the test. Viscosity testing has a normal variation of only 0.5%. In
contrast, the total base number (TBN) test has a variation of 15%. A reported TBN value of 7.0
could actually represent a value of between 5.95 and 8.05. The accuracy ranges have been
defined for the tests. Consult with the laboratory to account for variation in statistical trending
analysis. The value of the analytical test as an effective alarm trigger decreases as the test
variation increases.
The Total Base Number (TBN) can be described as a measure of an oils ability to neutralize
strong acids created during the combustion process. It is often referred to as the alkalinity of the
lubricant.
With many oils, the TBN value also gives an indication of the lubricant condition in terms of the
detergent additive concentration and therefore the level of detergency and dispersancy. Once a
new oil is put into service, the TBN will either slowly rise or fall from its new value to a value
known as the equilibrium TBN. This TBN level will remain fairly constant until the engine
operation conditions change. The fuel sulphur content and the oil consumption are among the
most influencing factors for the equilibrium TBN. For simplicity, we can say that a higher sulphur
fuel will cause a fall in TBN; an increase of the oil consumption would cause the TBN value to rise
while a reduction of the oil consumption would result in a lower equilibrium TBN.
Many engine OEMs specify the minimum equilibrium TBN of the used lubricant, in addition to
other parameters that should be carefully monitored in order to ensure the oil is in satisfactory
condition.

Analytical Ferrography
Analytical ferrography uses a high gradient magnetic field to attract and hold particles from a fluid
sample which flows down a specially prepared microscope substrate inclined at a small angle to
the horizontal. After preparation, the substrate is mounted on the microscope stage for optical
examination using a bichromatic microscope
Due to the intensive nature of this technique it is relatively expensive and only used when a
problem has already been highlighted by one of the trending techniques.

.
Figure 5 Equipment used in analytical ferrography#
Table 3 - Analytical Ferrography - capabilities