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Introduction to lubricants

Friction is the force that resists relative motion between two bodies in contact. If friction does not
exist, nothing would ever stop it moving. Therefore we need friction to function but we want to be
able to control the motion of moving parts at the same time, in order to reduce excessive friction.
When we rub our hands together, we create heat. It is because of the friction between the sliding
surfaces of hands. Now imagine rubbing hands together 3600 times a minute –hands would be on fire!
Similarly heat is generated by friction in machinery.
Mechanical Machines have moving, sliding or rolling, parts and during operation they rub against
each other. This mutual rubbing generates frictional force which offers resistance to the relative
motion of these surfaces. Wear and tear results when an external force is applied to overcome this
resistance resulting in replacement of mechanical parts.
Thus reducing friction and transferring heat to atmosphere are only two among a couple of
reasons we use lubricants.

Lubricants reduce friction and hence wear and tear between two moving metallic surfaces by
providing a thin film of continuously supplied fluid between them. They also act as cooling medium.
Suitable addition of chemicals can add the properties of sealing agents, corrosion including water
preventer, and carbon/sulphur solvent that bring desired long lasting results.
Lubrication is a process of introducing a substance called “lubricant” between two moving or
sliding surfaces to reduce friction between them.
The lubrication can act in following ways.

 Hydrodynamic or fluid film lubrication: Due to continuous rubbing of two metallic surfaces,
abrasion also takes place causing pieces of the weaker material to be grounded out in create finer
particles. Presence of these fine particles cumulatively increases more particles liberated due to
abrasion. It must be prevent from occurring and if occurred, these tiny particles must be swept out of
the circulation. This can be done if the lubricant fluid possesses the hydrodynamic and elasto-
hydrodynamic properties. In such type of mechanism two surfaces are separated from each other by
thick film of fluid. This mechanism is employed in light machines and in scientific instruments. It
uses hydrocarbon oils blended with long chain polymers to maintain the required viscosity.
 Thin film or boundary lubrication: These are the low viscosity lubricants employed in high load,
Low speed operations. Thin film lubricants use blended vegetable and animal oils.
 Extreme pressure lubrication: In condition like automobile gears, very high pressure at speed
generates excessive heat. Under such condition lubricants fails to stick to the moving surfaces. Hence
“special additives” are used to make lubricant stick to the surface. The additives include the use of
compounds of chlorine, sulphur and phosphorus.

On the basis of their physical state, lubricants are classified as:

Solid lubricants Semisolid lubricant liquid lubricant


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Additives: To improve the properties of the lubricating oils, certain substances called additives are
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added to the lubricating oils. The oils thus prepared are known as "Blended oils (or) Compounded
oils".
For example: Rust inhibitors protect surfaces against rust by forming a thin water repelling film on the
metals surface.
Dispersants help protect components against abrasion from wear by enveloping particles and
suspending them in the oil so that they may be easily flushed and removed from the system.
Anti-wear and extreme pressure (to reduce shear of the oil) additives react with a component’s
surfaces to form a thin protective layer to prevent metal-to-metal contact. This is especially helpful in
situations where there is high pressure or a lot of stop and start evolutions.
Detergents work to neutralize acids and clean surfaces where deposits may be detrimental. Finally,
foamant weakens the surface tension of bubbles so that they may break easily and minimize foaming.
In grease we use thickener. This is most commonly described as “the sponge that holds the lubricant.”
Up to thirty percent of grease is made up of the thickener which is either a simple or complex soap.
Simple soap is made up of long fibers and has a smooth, buttery texture. Examples of simple soaps
are lithium, poly-urea, calcium, and silica. Complex soap is made up of short and long fibers and has
a more fibrous texture. Some examples are aluminum, sodium, and barium.
Grease keeps contaminants out, is better suited for insoluble solid additives like molybdenum
disulfide and graphite, and has better stop-start performance because it doesn’t drain away like oil, for
a lower chance of a dry start. However, the thickness of grease limits bearing speed, reduces cooling
of components, makes for difficult sampling and analysis, and makes it difficult to determine the
proper amount of grease that needs adding. It must be taken into consideration when deciding if oil or
grease would be better suited for the application.

Some of the important additives used to enhance the property of lubricants are listed below
Any Lubricants must possess following properties. They should be
• Thermally stable at the operating temperature: The lubricants used should be thermally stable as it
may responsible for decrease in efficiency of machine and reduce functionality and working
capacity in decomposed form
.
• Chemically stable in corrosive environment: Chemical stability provides proper function of
lubricants in high temperature and pressure conditions. Chemically unstable lubricants reduce the
life of machinery.

• Possess high Viscosity Index (V.I.): As we know viscosity is very important characteristic
responsible for quality and selection of lubricants. A high viscosity index provides constant
viscosity over a wide range of temperature range.
• Possess high flash and fire point while low pour point: The lubricating oil used in various fields
should have high flash & fire point properties as it is responsible for safeguards against fire hazards.

• Reduce friction: When the two steel surfaces are separated by some lubricating oil, the small
peaks and valley do not interlock and thus by the use of lubricants we can reduce friction.

• Reduce wear: Direct contact between the sliding or moving surfaces is avoided so wear, tear and
surface deformation are reduced.

• Seal power: In an internal combustion engine the lubricant used between the piston and cylinder
wall act as a seal. This seal prevents the leakage of gases under high pressure from the cylinder.
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Important additives and their functions

Name of the Examples Functions Applications


additive
1. Oiliness Fatty acids such as They increase the oiliness or Added in machine used in
carriers. stearic acid, palmatic adhering property of boundary lubrication.
acid, oleic acid. lubricants.
2. Extreme Organic chlorine They react with metal surface Used in condition of high
pressure compounds, organic forming surface film of lower temperature and pressure in
additives. sulphur compounds, shear strength and high lubrication.
organic phosphorous melting point.
compounds.
3. Viscosity Polymers and co- They prevent the oil from Added in the machines
index polymers of olefins thining at higher temperatures working under broad range of
improvers. and thickening at lower temperature change.
temperatures.
4. Pour-point Alkylated naphthalene Lowers the pour point of the Reduce interlocking
depressants. and phenolic polymers , oil
polymethacrylates.
5. Thickeners Polyesters, polystyrene. They increase the viscosity of Used for forming greases.
the lubricants.
6. Antioxidants Aromatic phenolic and They retard the oxidation Added in lubricants used in
amino compounds of the oil and prevent the internal combustion engine.
formation of gum-like
substances.
8. Corrosion Organometallic Protect the metal in contact In lubricating oils used for
inhibitors. compounds , zinc dithio with the lubricants from bearings etc.
phosphates corrosion.

9. Flash & fire Triphenyl phosphate & They increases flash point of Used to enhance properties
point impruvers glycerol acetals lubricating oil

Synthetic lubricants: They are the lubricants that are prepared in laboratory. They are much better
than ordinary lubricants because they can work under extreme conditions. For example: - silicones,
chlorinated hydrocarbons, silicate esters etc. Biodegradable lubricants: They are those substances
which are able to decompose in nature. Environment in water, soil without yielding harmful
substances by action of micro- organism and also act as lubricants. They are typically vegetable oil
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based.
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To understand them, we conduct following experiments here in our laboratory.
• Viscosity and Viscosity Index (R.W.1&2)
• Flash and Fire Point (Abel’s, Pensky Martenes, Clevelands apparatus)
• Cloud and Pour point
• Aniline point
• Steam Emulsion Number
• Properties of grease by cone penetrometer

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REDWOOD VISCOMETER NO.1

1. Aim: Determine the change in viscosity of a given lubricating oil with change in temperature
by Redwood Viscometer No. 1
2. Objectives:
 What are lubricants
 Different types of functions performed by lubricants
 Types of lubricants
 Properties and mechanism of lubricants
 Viscosity & determination of viscosity index
 Significance of viscosity measurements and practical utility
3. Outcomes:
 Able to know basic properties of lubricants
 Significance of viscosity in engineering
 To know effect of temperature on lubricants
 Able to apply basic property in applied mechanis

4. Theory with self-assessment questionnaire and problem enunciation:


Viscosity: Viscosity is the measure of resistance of a fluid to deform under stress. It is commonly
known as thickness or resistance to flow. Viscosity describes a fluid internal resistance to flow
thus water is thin having a lower viscosity while vegetable oil is thick having a higher viscosity.
All fluids have resistance to flow but a fluid which has no resistance is known as ideal fluid.
Absolute viscosity is defined as the force in dynes necessary for the movement of 1 sq.cm layer of
a fluid with a velocity of 1cm/sec from another parallel layer 1 cm away. Absolute viscosity
values are required for use in all bearing design calculation and other lubrication engineering
technical design problems. Kinematic viscosity is defined as the ratio of absolute viscosity to
density. Kinematic values are applied in oil blending procedures under extreme condition when
additives are added.

Types and Units of viscosity:


• Dynamic/absolute viscosity: The IUPAC symbol for viscosity is eta (η) and dynamic
viscosity is also commonly referred to using the symbol mu (µ). The S.I. physical unit of
dynamic viscosity is pascal-secnd (Pa.s) equal to 1 kg.m-1.s-1 and N.S/m2 .The CGS unit for
dynamic viscosity is poise and centipoise and dyne.s/cm2
Thus 10P = 1 kg.m-1.s-1 = 1Pa.s
• Kinematic viscosity: Kinematic viscosity has SI unit m2.s-1. The CGS unit for kinematic
viscosity is the stokes (St) and also expressed as centistokes (cSt).

Self assesment 1:
1. Define lubricants.
2. Describe various functions and properties of lubricants
3. What do you mean by additives and why it is used?
4. Define viscosity of lubricating oil.
5. Why viscosity is important in lubrication?
6. With increase of pressure viscosity also increases why?
7. Define function of valve rod in apparatus
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8. Why we use water bath in apparatus can it works without water bath?
9. Describe synthetic and biodegradable lubricants.

Effect of temperature and pressure on viscosity:


• Viscosity is inversely proportional to temperature. This is due to decrease in intermolecular
attraction between the lubricating oil.
• Viscosity is directly proportional to pressure. This is due to the increase in intermolecular
attraction between the lubricating oil.

Viscosity Index: It is a lubricating oil quality indicator, an arbitrary measure for the change of
kinematic viscosity with temperature thus “the rate at which viscosity of lubricant changes with
temperature is measured by an arbitrary scale known as viscosity index (V.I.)For determining
viscosity index two types of references are used. One of these is pennysylvanian oils consist
mainly of paraffins and show small decrease in viscosity with increase in temperature having V.I.
= 100.The other reference taken is gulf oils consist of alicyclic hydrocarbons and have large
variation in viscosity with temperature with V.I. = 0.

V.I. = 100 (For Pennysylvanian oils)


V.I. = 0 (For Gulf oils)
Viscosity Index= VL – U/VL–VH X 100
VL =viscosity at 1000F of gulf oil, U = viscosity of oil under test at 1000F.
VH = viscosity at 1000F of pennysylvanian oil.
Higher the V. I., lower the variation of viscosity with change in temperature.
There are different types of chemicals used as viscosity index improver, which can sufficiently
increase viscosity index of particular oil. Polymers and copolymers of olefin, silicones (SiO2),
polyglycol ethers and diesters mainly used as V.I. improve

self assesment 2:
10. What do you mean by absolute and kinematic viscosity
11. Why on increase of temperature viscosity decreases
12. What do you mean by V.I.
13. Which two standard oils used as a reference in determining V.I. explain chemical
composition.
14. If V.I. = 100 & 0 than what does it means?
15. If there is sudden change in viscosity with temperature then what you will conclude?
16. Explain significance of the experiment.

Viscosity test: Generally four viscometers are used to measure the viscosity of fluids
• Redwood Viscometer
• EnglerViscometer
• Saybolt Viscometer
• Kinematic Viscometer
5. Precautions:
1. The oil should be filtered through a muslin cloth to remove solid particles that may
clog the jet.
2. The receiving flask should be placed in such a way that the oil stream from the jet
stokes the neck of receiving flask and does not cause foaming.
3. After each reading the oil should be completely drained out of the receiving flask.
6. Experimental setup
Description of setup
There are two types of Redwood viscometers i.e.Redwood viscometer No.1 and No.2. The two
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viscometers work on same principle, and have same shape and method of testing. The only
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difference lies in the dimensions of the discharge capillary.


Redwood viscometer No. 1 is commonly used for determining the viscosities of thin lubricating
oils [kerosene , mustard oil; etc ]as it has smaller jet diameter of 1.62 mm with a length 10
mm. Redwood viscometer No. 2 is used for determining the viscosities of highly viscous
oils [mobile oil , glycerol etc. ] and has jet diameter of 3.8 mm and length 50 mm.
Redwood viscometer consists of the following parts:
Oil cup: It is a silver – plated brass cylinder having height of 90 mm and a diameter of
46.5 mm. The bottom of the cup is provided with a central hole in which an agate jet with
bore diameter 1.62 mm and length 10 mm is fitted. This jet can be opened / closed by a valve
rod. To indicate the level to which the cylinder is to be filled with oil, a pointer is fixed on
the inner side of the cylinder. The pointer is a stout, tapered, upward-pointing wire. A
thermometer is inserted in the cup through the lid of the cup.
Heating bath: A cylindrical copper bath containing water surrounds the oil cup. A thermometer
is also inserted in the copper bath to know the temperature of water. Heating bath is also
provided with a stirrer for stirring the water to keep the Temperature of water uniform
throughout. The stirrer is provided with a circular shield to prevent any water splashing
into the cylinder.
Spirit level: A spirit level used for leveling the apparatus vertically is also provided in
the lid of the cup. The entire apparatus is supported on three legs, provided at the bottom
with leveling screws.
Kohlrausch flask: A specially shaped flask known as kohlrausch flask is provided to
receive the oil from the outlet. The flask is of 50 ml capacity.
7. Procedure:
1. Clean the cylindrical oil cup and ensure the orifice tube is free from dirt .
2. Close the orifice with ball valve.
3. Place the 50 ml flask below the opening of the Orifice .
4. Fill the oil in the cylindrical oil cup upto the mark in the cup .
5. Fill the water in the water bath.
6. Insert the thermometers in their respective places to measure the oil and water bath
temperatures.
7. Heat the by heating the water bath, Stirred the water bath and maintain the uniform
temperature .
8. At particular temperature lift the bal valve and collect the oil in the 50 ml flask and note the
time taken in seconds for the collecting 50 ml of oil. A stop watch is used measure the time
taken . This time is called Redwood seconds.
9. Increase the temperature and repeat the procedure ‘8’ and note down the Redwood seconds
for different temperatures.

8. Bill of Material: Redwood Viscometer No.1, stop watch, given oil sample, thermometers,
receiving flask, water etc.
9. Expectations
1. Experiment should be clearly performed according to temperature condition.
2. Stirring should be proper for equal distribution of temperature.
3. Must maintain temperature of oil cup and water bath.
4. Graph plotted and diagram drawn should be neat and clean.
5. Reading obtained must follow temperature condition.
Students are expected to submit the following in their own handwriting and style:
1. Self assessment questions with reasoning.
2. Neat and clean labeled diagram as well as graph.
3. Result and justification of result should be in agreement with problem statement.
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10. Observation Table:
S.No. Volume of oil sample Temperature(ᵒC) Viscosity (Time in sec.
Water Oil for flow of 50ml of oil)
1
2
3
4
5

“Graph: The following graph has to be drawn


Temperature Vs Redwood seconds”

RESULT: The graph represents that ________________________

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REDWOOD VISCOMETER NO.2

1. Aim: Determine the change in viscosity of a given lubricating oil with change in temperature by
Redwood Viscometer No. 2
2. Objectives:
 What are lubricants
 Different types of functions performed by lubricants
 Types of lubricants
 Properties and mechanism of lubricants
 Viscosity & determination of viscosity index
 Significance of viscosity measurements and practical utility
3. Outcomes:
 Able to know basic properties of lubricants
 Significance of viscosity in engineering
 To know effect of temperature on lubricants
 Able to apply basic property in applied mechanism

4. Theory with self-assessment questionnaire and problem enunciation:


Viscosity: Viscosity is the measure of resistance of a fluid to deform under stress. It is commonly
known as thickness or resistance to flow. Viscosity describes a fluid internal resistance to flow thus
water is thin having a lower viscosity while vegetable oil is thick having a higher viscosity. All fluids
have resistance to flow but a fluid which has no resistance is known as ideal fluid.
Absolute viscosity is defined as the force in dynes necessary for the movement of 1 sq.cm layer of a
fluid with a velocity of 1cm/sec from another parallel layer 1 cm away. Absolute viscosity values are
required for use in all bearing design calculation and other lubrication engineering technical design
problems.
Kinematic viscosity is defined as the ratio of absolute viscosity to density. Kinematic values are
applied in oil blending procedures under extreme condition when additives are added.
Lubricants used between moving piston and the cylinder wall of an I.C. engine also acts as a seal
between them, thereby preventing the leakage of gases under high pressure from the cylinder.

Types and Units of viscosity:


• Dynamic/absolute viscosity: The IUPAC symbol for viscosity is eta (η) and dynamic viscosity is
also commonly referred to using the symbol mu (µ). The S.I. physical unit of dynamic viscosity is
pascal-secnd (Pa.s) equal to 1 kg.m-1.s-1 and N.S/m2 .The CGS unit for dynamic viscosity is poise
and centipoise and dyne.s/cm2
Thus 10P = 1 kg.m-1.s-1 = 1Pa.s
• Kinematic viscosity: Kinematic viscosity has SI unit m2.s-1. The CGS nit for kinematic viscosity is
the stokes (St) and also expressed as centistokes (cSt).

Self assesment 1:
1. Define difference between Redwood Viscometer No.1 &2?
2. Describe various types of Viscometers used to determine viscosity.
3. What do you mean by thick film lubrication?
4. Why thin film is called boundary lubrication?
5. How extreme pressure lubricants work?
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6. Capacity of kohlrausch flask is ………………


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7. Define solid lubricants with examples.


8. Why grease is called semisolid lubricants?
9. Solid lubricants used in what type of condition?
Effect of temperature and pressure on viscosity:
• Viscosity is inversely proportional to temperature. This is due to decrease in intermolecular
attraction between the lubricating oil.
• Viscosity is directly proportional to pressure. This is due to the increase in intermolecular
attraction between the lubricating oil.
Viscosity Index: It is a lubricating oil quality indicator, an arbitrary measure for the change of
kinematic viscosity with temperature thus “the rate at which viscosity of lubricant changes with
temperature is measured by an arbitrary scale known as viscosity index (V.I.)For determining
viscosity index two types of references are used. One of these is pennysylvanian oils consist mainly of
paraffins and show small decrease in viscosity with increase in temperature having V.I. = 100.The
other reference taken is gulf oils consist of alicyclic hydrocarbons and have large variation in
viscosity with temperature with V.I. = 0.
V.I. = 100 (For Pennysylvanian oils)
V.I. = 0 (For Gulf oils)
Viscosity Index= VL – U/VL–VH X 100
VL =viscosity at 1000F of gulf oil, U = viscosity of oil under test at 1000F.
VH = viscosity at 1000F of pennysylvanian oil.
Higher the V. I., lower the variation of viscosity with change in temperature.
There are different types of chemicals used as viscosity index improver, which can sufficiently
increase viscosity index of particular oil. Polymers and copolymers of olefin, silicones (SiO2),
polyglycol ethers and diesters mainly used as V.I. improver.
There are four types of lubricants generally used in solid form in lubrication graphite, MoS 2,
soapstone and mica.
self assesment 2:
10. What do you mean by zero viscosity?
11. What do you mean by SAE viscosity grade?
12. How viscosity index improver works.
13. Why we can’t use petrol in diesel engine and vice versa?
14. Name any three types of solid lubricants?
15. Give an example in which lubricants also act as a seal?
16. Why does graphite act as a good lubricant on the surface of moon?
Viscosity test: Generally four viscometers are used to measure the viscosity of fluids
• Redwood Viscometer
• EnglerViscometr
• Saybolt Viscometer
• Kinematic Viscometer
“Temperature on moon is 110̊ C during day time and -150̊ C during nights. So oil or grease
cannot act as a lubricant under these conditions. On the other hand, a solid lubricant like graphite
is very little affected by temperature changes. Hence, graphite acts as a good lubricant on the
surface of moon”.
5. Precautions:
1. The oil should be filtered through a muslin cloth to remove solid particles that may
clog the jet.
2. The receiving flask should be placed in such a way that the oil stream from the jet
stokes the neck of receiving flask and does not cause foaming.
3. After each reading the oil should be completely drained out of the receiving flask.
6. Experimental setup
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Description of setup
There are two types of Redwood viscometers i.e.Redwood viscometer No.1 and No.2. The two
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viscometers work on same principle, and have same shape and method of testing. The only difference
lies in the dimensions of the discharge capillary.
Redwood viscometer No. 1 is commonly used for determining the viscosities of thin lubricating oils
[kerosene , mustard oil; etc ]as it has smaller jet diameter of 1.62 mm with a length 10 mm.
Redwood viscometer No. 2 is used for determining the viscosities of highly viscous oils
[mobile oil , glycerol etc. ] and has jet diameter of 3.8 mm and length 50 mm.
Redwood viscometer consists of the following parts:
Oil cup: It is a silver – plated brass cylinder having height of 90 mm and a diameter of 46.5
mm. The bottom of the cup is provided with a central hole in which an agate jet with bore
diameter 3.82 mm and length 50 mm is fitted. This jet can be opened / closed by a valve rod. To
indicate the level to which the cylinder is to be filled with oil, a pointer is fixed on the inner
side of the cylinder. The pointer is a stout, tapered, upward-pointing wire. A thermometer is
inserted in the cup through the lid of the cup.
Heating bath: A cylindrical copper bath containing water surrounds the oil cup. A thermometer is
also inserted in the copper bath to know the temperature of water. Heating bath is also
provided with a stirrer for stirring the water to keep the Temperature of water uniform
throughout. The stirrer is provided with a circular shield to prevent any water splashing into
the cylinder.
Spirit level: A spirit level used for leveling the apparatus vertically is also provided in the
lid of the cup. The entire apparatus is supported on three legs, provided at the bottom with
leveling screws.
Kohlrausch flask: A specially shaped flask known as kohlrausch flask is provided to receive
the oil from the outlet . The flask is of 50 ml capacity.
7. Procedure:
1. Clean the cylindrical oil cup and ensure the orifice tube is free from dirt .
2. Close the orifice with ball valve.
3. Place the 50 ml flask below the opening of the Orifice .
4. Fill the oil in the cylindrical oil cup upto the mark in the cup .
5. Fill the water in the water bath.
6. Insert the thermometers in their respective places to measure the oil and water bath
temperatures.
7. Heat the by heating the water bath, Stirred the water bath and maintain the uniform
temperature .
8. At particular temperature lift the bal valve and collect the oil in the 50 ml flask and note the
time taken in seconds for the collecting 50 ml of oil . A stop watch is used measure the time
taken . This time is called Redwood seconds.
9. Increase the temperature and repeat the procedure ‘8’ and note down the Redwood seconds
for different temperatures.

8. Bill of Material: Redwood Viscometer No.2, stop watch, given oil sample, thermometers,
receiving flask, water etc.

9. Expectations
1. Experiment should be clearly performed according to temperature condition.
2. Stirring should be proper for equal distribution of temperature.
3. Must maintain temperature of oil cup and water bath.
4. Graph plotted and diagram drawn should be neat and clean.
5. Reading obtained must follow temperature condition.
Students are expected to submit the following in their own handwriting and style:
1. Self assessment questions with reasoning.
2. Neat and clean labeled diagram as well as graph.
3. Solved tutorial problem and value addition questions.
4. Result and justification of result should be in agreement with problem statement.
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10. Observation Table:
S.No. Volume of oil sample Temperature(ᵒC) Viscosity (Time in sec.
Water Oil for flow of 50ml of oil)
1
2
3
4
5

“Graph: The following graph has to be drawn


Temperature Vs Redwood seconds”

RESULT: The graph represents that ________________________

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FLASH AND FIRE POINT

Flash Point It is the lowest temperature at which the oil gives off enough vapour that ignites for a
moment, when a small flame is brought near it.
Fire Point It is the lowest temperature at which the vapour of the oil burns continuously for at least 5
seconds, when a small flame is brought near it. Generally the fire point is 5-40°C higher than flash
point.
Auto ignition A material's auto ignition or ignition temperature is the temperature at which a material
self-ignites without any obvious sources of ignition, such as a spark or flame. Most common
flammable and combustible liquids have auto ignition temperatures in the range of 300°C (572°F) to
550°C (1022°F).
Auto ignition
Fuel Flash point
temperature
Gasoline (petrol) −43 °C (−45 °F) 280 °C (536 °F)
Diesel (2-D) >52 °C (126 °F) 256 °C (493 °F )
Ethanol (70%) 16.6 °C (61.9 °F) 363 °C (685 °F)
Jet fuel >60 °C (140 °F) 210 °C (410 °F)
Kerosene (paraffin) >38–72 °C (100–162 °F) 220 °C (428 °F)
Vegetable oil (canola) 327 °C (621 °F)
Biodiesel >130 °C (266 °F)
Measurement of flash and fire points of a lubricating oil by different types of apparatus.

Cleveland open cup-All Petroleum Products except fuel oils.(above 790C or 1750f)

Pensky Martin Closed cup Apparatus-lubricating oils, fuel oils, solvents, solvent containing
materials. (50 to 3700 C or 1200f to 6980f)

Abel’s closed cup Apparatus-inflammable oils, fuel oils. (Up to 490C or below 1200f)

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PENSKY MARTEN’S APPARATUS

1. Aim : To determine Flash Point of given lubricating oil by Pensky Marten Apparatus.
2. Objectives:
 What is flash point?
 Why we determine flash point.
 Significance of flash point determination.
 How it affects working of lubricating oil.
3. Outcomes:
 Able to know basic properties of lubricants
 Significance of flash point in engineering.
 Safeguards against fire hazards.
 Able to apply basic property in applied mechanism

4. Theory with self-assessment questionnaire and problem enunciation:


Flash Point is the lowest temperature at which the lubricating oil gives off enough Vapors
that ignite for a moment when a tiny flame is brought near it. Fire Point is the Lowest
temperature at which the vapors of the oil burn continuously for at least five seconds When a
tiny flame is brought near it.. Contaminated coolant can cause deterioration of metal components in
the radiator, heater core, engine block, plugs and thermostat. Rubber components such as hoses and
gaskets react by leaking, causing coolant loss, resulting in overheating and engine failure.
Contamination with small amounts of volatile: Because of their presence irregular flashes can be
observed below the true flash point of lubricating oil. It is called “freaky flash point”
Self assessment: 1
1. What do you mean by flash & fire point?
2. What is the utility of flash point determination?
3. What is temperature difference between flash point and fire point?
4. Describe three types of apparatus used to determine flash and fire points and also difference
between them.
5. For safe use, flash point & Fire point of lubricant oil should be………………..
6. What do you mean by Auto ignition Temperature?
7. What do you mean by freaky flash?

Significance: Good lubricating oil should have flash and fire points higher than the operating
temperature of the machine. A knowledge of flash and fire point is useful in providing protection
against fire hazard during transport and storage. Lubricating oils of paraffinic base possess higher
flash points than those of naphthenic base. Hence the determination of flash and fire points is
helpful in identifying the type of lubricating oil and gives following information.
 Fire hazard of petroleum products and evaporation loses under high temperature loses
 It gives us the idea about the maximum temperature below which the oil can be used
 It is used as the means of identification of specific lubricating oil
 For detection of contamination in the given lubricating oil
Flash point of lubricant is lower if it contains low molecular weighthydrocarbons. If moisture is
present in the lubricating oil it increases the flash point because steam prevents vapour from ignition.

self assesment 2:
8. Define function of air bath in Pensky marten’s apparatus.
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9. What is use of stirrer and what are the number of blades in stirrer in Pensky martins
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10. Which type of lubricants use in this apparatus?


11. Define additives and type of additives used to increase flash & fire points of lubricating oil.
12. Is change in flash point also indicate contamination?
13. Describe significance of experiment.
14. Name the impurities which can increase or decrease the flash point of lubricating oil.
5. Precautions:
1. The apparatus should be thoroughly dried because the moisture affects the flash point as
steam prevents vapours from igniting.
2. The thermometer bulb should dip into the oil.
3. For introducing the flame the shutter should be drawn open slowly and closed
quickly.While applying the test flame, stirring should be discontinued
6. Experimental setup
Description of setup
It consists of Following parts:-
Oil Cup : The oil cup made up of brass is about 5 cm in diameter and 5.5 cm deep. It
has a marking inside to indicate the level upto which the cup is filled. The lid of the cup
is provided with four openings. Through one opening, a thermometer is inserted while a
stirrer passes through the other , carrying two brass blades . The third opening is for
introducing a test flame and the fourth one is for introducing the air .
Shutter: The lid is provided with a shutter which can be moved to introduce the flame
when required .
Flame exposure device: It is a device for introducing a standard flame. It is connected to the
shutter in such a way that when the shutter is turned , openings of the test flame
exposure device dips into the opening over the surface of the oil .
Air bath : The oil cup is supported by its flange over air bath which is heated by a gas
burner.
Pilot Burner: Pilot burner lights the test flame which gets extinguished when it is
introduced into the opening for the test . The moment test flame returns to the original
position, pilot burner lights it.

7. Procedure:
1. Clean and dry all parts of the apparatus with the help of suitable solvent e.g. CCl 4, ether,
petroleum spirit or benzene and dry it to remove any traces of solvent.
2. Fill the oil cup with the test oil up to the mark.
3. Fix the lids on the top through which are inserted a thermometer and a stirrer. Ensure that the
flame exposure device is fixed on the top.
4. Light the test flame and adjust it to about 4 mm in diameter.
5. Heat apparatus as temp. of oil increases by 5 to 60 per min. as stirrer is continuously rotated.
6. At every 10ᵒC rise of temp. Introduce test flame into the oil vapor. This is done by operating the
shutter. On moving knob of shutter, test flame is lowered in oil vapors through opening.
7. When test flame causes a distinct flame in interior cup, note temp. which represent the flash point
8. Further heat the oil at the rate of 10ᵒC/ min. and continue applying the test flame as before.
9. The temperature at which the vapors of the oil givea clear and distinct blue flash for five seconds is
recorded as the fire point of the oil.

8. Bill of Material: Pensky Marten’s apparatus, given sample of oil, thermometer, thermostat,
Match box etc.
9. Expectations
1. Experiment should be clearly performed according to temperature condition.
2. Stirring should be proper for equal distribution of temperature.
3. Must maintain temperature of oil cup and regulate shutter opening accordingly.
15

4. Reading obtained must follow temperature condition.


Students are expected to submit the following in their own handwriting and style:
Page

1. Self assessment questions with reasoning.


2. Neat and clean labeled diagram.
3. Readings should be in agreement with increasing and decreasing temperature.
4. Result and justification of result should be according to problem statement.
10. Obsevation Table : (On Heating)
S. No. Temperature (0C) Observation Inference
1
2
3
4
5
6
7 Flash Observed Flash Point

(On Cooling)
S. No. Temperature (0C) Observation Inference
1
2
3
4
5

RESULT: The flash point of given oil sample =_______ 0C.

16
Page
ABEL’S CLOSED CUP APPARATUS

1. Aim: To determine Flash Point of given lubricating oil by Abel’s Apparatus.


2. Objectives:
 What is flash point?
 Why we determine flash point.
 Significance of flash point determination.
 How it affects working of lubricating oil.
 Difference between Pensky martins and able’s apparatus
3. Outcomes:
 Able to know basic properties of lubricants
 Significance of flash point in engineering.
 Safeguards against fire hazards.
 Able to apply basic property in applied mechanism
 Effect of contamination on properties of lubricating oil
4. Theory with self-assessment questionnaire and problem enunciation:
Flash Point is the lowest temperature at which the lubricating oil gives off enough Vapors
that ignite for a moment when a tiny flame is brought near it. Fire Point is the Lowest
temperature at which the vapors of the oil burn continuously for at least five seconds When a
tiny flame is brought near it.. Contaminated coolant can cause deterioration of metal components in
the radiator, heater core, engine block, plugs and thermostat. Rubber components such as hoses and
gaskets react by leaking, causing coolant loss, resulting in overheating and engine failure. There are
various types of factors that affect flash and fire points as frequency of application of test flame, rate
of heating, rate of stirring, size of test flame and time of opening the shutter.

Self assessment: 1
1. Explain difference between Ables and Pensky Marten’s apparatus for flash point
determination?
2. What is difference between flammable & combustible liquid?
3. Which apparatus gives best result in order to determine flash & fire point?
4. How moisture is removed from lubricating oil?
5. What are the factors that affects flash & fire point?
6. What are the types of lubricants used in Abel’s apparatus?
7. Define temperature range used in Able’s apparatus.
8. Can you determine flash point of lubricants which we observe through pensky martins?

Significance: Good lubricating oil should have flash and fire points higher than the operating
temperature of the machine. A knowledge of flash and fire point is useful in providing protection
against fire hazard during transport and storage. Lubricating oils of paraffinic base possess higher
flash points than those of naphthenic base. Hence the determination of flash and fire points is helpful
in identifying the type of lubricating oil and gives following information.
 Fire hazard of petroleum products and evaporation loses under high temperature loses
 It gives us the idea about the maximum temperature below which the oil can be used
 It is used as the means of identification of specific lubricating oil
 For detection of contamination in the given lubricating oil
17

Abel’s closed cup apparatus can be used to determine flash point bellow 0ᵒC as inspite of heating the
Page

oils it canbe cooled by using liquid NH3 and solid CO2.


Self assessment: 2
9. What are additives? Define function of additives
10. What is mode of heating in Able’s apparatus
11. Define thermostat
12. Why we observe temperature in both conditions(increasing and decreasing)
13. Describe use of stirrer in apparatus.
14. Is shutter opening time affects flash point of lubricant?
15. Why we avoid sudden increase or decrease of temperature in thermostat.
16. Is it possible to determine the flash point below 0ᵒC?Which apparatus is used for that.

5. Precautions:
1. The apparatus should be thoroughly dried because the moisture affects the flash point as
steam prevents vapours from igniting.
2. The thermometer bulb should dip into the oil.
3. For introducing the flame the shutter should be drawn open slowly and closed quickly.
4. While applying the test flame, stirring should be discontinued.
6. Experimental setup
Description of setup
Abel’s closed cup apparatus: It consists of following parts:-
Abel’s apparatus essentially consist of a cylindrical brass cup surrounded by a double jacketed
copper water bath which is enclosed in a copper casing mounted on iron tripod. The space between
the water bath & the oil cup form an air bath by means of which the oil can be heated uniformly.
The oil cup is provided with a brass cover having arrangement for a small test flame, a sliding
shutter covering three small opening in the lid & opening for a paddle stirrer & a standard
thermometer, the bulb of which should be immersed in the oil. When the shutter is open, the test
meets the ascending current of oil vapour & air while at the same time atmospheric air passes into
the two smaller side openings. A bent gauge terminating with a point ending indicates the depth to
which the oil must be filled into the cup. The apparatus is provided with an electrical heating device
connected to rheostat.
7. Procedure:
1. Clean and dry all parts of the apparatus with the help of suitable solvent e.g. CCl 4, ether,
petroleum spirit or benzene and dry it to remove any traces of solvent.
2. Fill the oil cup with the test oil up to the mark.
3. Fix the lids on the top through which are inserted a thermometer and a stirrer. Ensure that the
flame exposure device is fixed on the top.
4. Light the test flame and adjust it to about 4 mm in diameter.
5. Heat apparatus as temp. of oil increases by 5 to 60per min. as stirrer is continuously rotated.
6. At every 10C rise of temp. Introduce test flame into the oil vapor. This is done by operating the
shutter. On moving knob of shutter, test flame is lowered in oil vapors through opening.
7. When test flame causes a distinct flame in interior cup, note temp. which represent the flash
point.
8. Further heat the oil at the rate of 10C/ min. and continue applying the test flame as before.
9. The temperature at which the vapors of the oil givea clear and distinct blue flash for five seconds
is recorded as the fire point of the oil.

8. Bill of Material: Able’s apparatus, given sample of oil, thermometer, thermostat, Match Box
etc.
18

9. Expectations
Page

1. Experiment should be clearly performed according to temperature condition.


2. Stirring should be proper for equal distribution of temperature.
3. Must maintain temperature of oil cup and regulate shutter opening accordingly.
4. Reading obtained must follow temperature condition.
Students are expected to submit the following in their own handwriting and style:
1. Self assessment questions with reasoning.
2. Neat and clean labeled diagram.
3. Prepare value addition questions.
4. Result and justification of result should be in agreement with problem statement.

10. Observation Table: (On Heating)


S. No. Temperature (0C) Observation Inference
1
2
3
4
5
6
7 Flash Observed Flash Point

(On Cooling)
S. No. Temperature (0C) Observation Inference
1
2
3
4
5

RESULT: The flash point of given oil sample =_______ 0C.

19
Page
CLEVELAND APPARATUS

1. Aim : To determine Flash Point of given lubricating oil by Cleveland Apparatus.


2. Objectives:
 What is flash point?
 Why we determine flash point.
 Significance of flash point determination.
 How it affects working of lubricating oil.
 To know difference between open & closed cup apparatus
3. Outcomes:
 Able to know basic properties of lubricants
 Significance of flash point in engineering.
 Safeguards against fire hazards.
 Able to apply basic property in applied mechanism
 Importance and use of different type of apparatus and their significance.

4. Theory with self-assessment questionnaire and problem enunciation:


Flash Point is the lowest temperature at which the lubricating oil gives off enough Vapors
that ignite for a moment when a tiny flame is brought near it. Fire Point is the Lowest
temperature at which the vapors of the oil burn continuously for at least five seconds When a
tiny flame is brought near it.. Contaminated coolant can cause deterioration of metal components in
the radiator, heater core, engine block, plugs and thermostat. Rubber components such as hoses and
gaskets react by leaking, causing coolant loss, resulting in overheating and engine failure. There are
various types of factors that affect flash and fire points as frequency of application of test flame, rate
of heating, rate of stirring, size of test flame and time of opening the shutter.This apparatus is used to
determine the flash and fire point of all petroleum products except fuel oil having an open cup flash
below 120̊C.Breathing should be avoided over oil cup as it may contain various types of harmful
evaporations.
Vapoursgenerally composed of low molecular weight hydrocarbons like H2, CH4 andC2H4. In
cleveland’s apparatus oil gets filled up to the mark because the space above oil act as an energy
barrier for the molecules of vapour which give flash.
Self assessment: 1
1. Why Cleveland is called open cup apparatus?
2. Is Cleveland is better as compared to rest two closed cup apparatus?
3. Explain types of lubricants used in cleveland apparatus.
4. Describe difference between open and closed cup apparatus.
5. What is the constitution of vapors which gives flash?
6. Why the oil in cleveland’s apparatus is filled up to the mark?

Significance: Good lubricating oil should have flash and fire points higher than the operating
temperature of the machine. A knowledge of flash and fire point is useful in providing protection
against fire hazard during transport and storage. Lubricating oils of paraffinic base possess higher
flash points than those of naphthenic base. Hence the determination of flash and fire points is helpful
in identifying the type of lubricating oil and gives following information.For domestic purpose flash
point above 50̊C is not desirable. Vapor pressure is an indication of a liquid'sevaporation rate. It
relates to the tendency of particles to escape from the liquid (or a solid). A substance with a high
20

vapor pressure at normal temperatures is often referred to as volatile.


 Fire hazard of petroleum products and evaporation loses under high temperature loses
Page

 It gives us the idea about the maximum temperature below which the oil can be used
 It is used as the means of identification of specific lubricating oil
 For detection of contamination in the given lubricating oil

Self assessment: 2
7. Why we get higher flash point than the actual one by this method.
8. Can we get accurate flash point by this method?
9. For domestic purpose flash point of which temperature is not desirable?
10. What do you mean by vapor pressure of the liquid?
11. Why we about breathing over oil cup?

5. Precautions:
1. The laboratory should be free from air drafts
2. Heating device must be switched off after determination
3. Breathing over the surface of the oil should be avoided.
6. Experimental setup
Description of setup
Cleveland open cup apparatus: It consists of following parts:-
Oil cup: The apparatus consist of a brass cup with a mark showing the level upto which the oil
should be filled.
Board: A board is there in the apparatus with a circular hole at the center in which the cup is fitted.
Base of the cup: The cup is supported by a metal plate which has a circular opening at the center,
of enough size to fit the cup in position.
Heating device: An electrical heating device is provided in such a way that the cup is uniformly
heated.
Clamp: A clamp is provided to hold the thermometer.
Thermometer: Thermometer of range 0-400 ̊C used with the apparatus.
7. Procedure:
1. The cup is filled with the oil under test in such a way that the oil level is exactly up to the mark.
2. The thermometer is held vertically by means of the clamp such that the bottom of the bulb is not
touch the bottom of the cup .
3. Heating is started by electrical device and the rise in temperature observed with the help of
thermometer.
4. At every degree rise in temperature the test flame is brought near the mouth of the opening of the
oil cup and observed whether a flash appear on oil surface.
5. The minimum temperature at which the distinct flash appears on the surface of the oil is recorded
as the flash of the oil.
6. Procedure is repeated by cooling the oil and results are reported by comparing both observation
table.

8. Bill of Material: Cleveland apparatus, given sample of oil, thermometer, thermostat, Match Box. e
9. Expectations
1. Experiment should be clearly performed according to temperature condition.
2. Stirring should be proper for equal distribution of temperature.
3. Must maintain temperature of oil cup and regulate shutter opening accordingly.
4. Reading obtained must follow temperature condition.
Students are expected to submit the following in their own handwriting and style:
1. Self assessment questions with reasoning.
2. Neat and clean labeled diagram.
3. Prepare value addition questions.
21

4. Result and justification of result should be in agreement with problem statement.


Page
10. Observation Table: (On Heating)
S. No. Temperature (0C) Observation Inference
1
2
3
4
5
6
7 Flash Observed Flash Point

(On Cooling)
S. No. Temperature (0C) Observation Inference
1
2
3
4
5

RESULT: The flash point of given oil sample =_______ 0C.

22
Page
CLOUD AND POUR POINT

1. Aim: Determine Cloud & Pour Point of given lubricating oil by Cloud & Pour Point Apparatus.
2. Objectives:
 What is cloud point?
 What is pour point?
 Why we determine cloud and pour point.
 Significance of cloud and pour point determination.
 How it affects working of lubricating oil.
3. Outcomes:
 Able to know basic properties of lubricants
 Significance of cloud and pour point in engineering.
 Safety against jamming of machine.
 Able to apply basic property in applied mechanism.
 Able to know effect of additives
4. Theory with self-assessment questionnaire and problem enunciation:
When an oil is cooled slowly, the temperature at which it becomes cloudy or hazy is called
cloud point, while the temperature at which the oil ceases to flow or pour is called Pour
point. Lubricating oil derived from petroleum usually contain dissolved paraffin wax and other
asphalted and resinous impurities, their amount depends on the refining process used. These
impurities tend to separate out from the oil at lower temperature. When petroleum oil is cooled under
specified condition at a specified rate the temperature at which crystallization of solids occur in the
form of cloud or haze, known as cloud point. The cooling is continued further, the amount of
separating matter increases and a stage is reached when this oil just ceases to flow. This temperature
is known as pour point.

Freezing Mixture: a combination of substances that when mixed lower the temperature of the
mixture by absorbing the melting heat or the heat of solution of the system’s components, which can
be liquid, solid, or both. To attain the lowest possible temperature, the components of a freezing
mixture are used in quantities that will form a cryohydrate. Water, ice, snow, and various salts and
acids will form freezing mixtures that attain a temperature of — 50°C.
Freezing mixtures commonly used for temperatures down to those shown are as follows:
 Ice and water 9°C
 Crushed ice and sodium chloride crystals −12°C
 Crushed ice and calcium chloride crystals −27°C
 Acetone or petroleum naphtha chilled −57°C
Self assessment: 1
1. What are lubricants?
2. Define cloud and pour point of liquid lubricants?
3. What do you mean by freezing mixture, give example and define function of freezing mixture?
4. How cloud and pour point of any lubricating oil disturb the safe working of the machine in
which it’s been used.
5. How cloud point gets increased or decreased of given oil.
23

6. Why separation of test tube from apparatus should be avoided during reading observation.
7. How paraffin wax in lubricating oil affect cloud and pour point.
Page

Significance: Most of the petroleum oils do not have fixed freezing point because they are mixtures
of various compounds. When lubricating oil is allowed to cool slowly, it starts appearing cloudy.
Cloud and pour point has great significance of indication of oils applicability and suitability in cold
conditions (low temperature).
There are two types of chemical reactions occurs in oil tube and in freezing mixture
Oil tube-Exothermic reaction
Freezing mixture- Endothermic reaction
 Most of the petroleum based lubricating oils contain dissolved paraffin wax and asphaltic
impurities. When the oil is cooled these impurities undergo solidification which cause jamming of
the machine.
 So the cloud and pour points indicate the suitability of the lubricants in cold condition.
 A good lubricant must have low cloud point and pour point.
 The lubricating oils used in the capillary feed systems should have low pour points, otherwise at
low temperatures the crystals of impurities will separate out clogging the capillary.
 In the fuel intake system of diesel engine, the lubricants having high cloud points may clog the
filter screens.
Self assessment: 2
8. What is use of air jacket in this experiment?
9. What is diameter of test tube used in apparatus?
10. Name different types of pour point depressants used in lubricating oil
11. Define significance of cloud and pour point.
12. Is cloud and pour point only important with respect to safe working?
13. Cloud and pour point should be higher or lower than working temperature.
14. Why we add salt over ice layer does it affect melting?
15. Which type of reaction occurs in oil tube and freezing mixture?
5. Precautions:
1. The complete operation of the removal and replacement of the test jar should be completed
within 3 seconds.
2. When the separation of the wax starts, care should be taken not to disturb the mass of the oil.
3. If the pour point is very low, a number of freezing mixtures with decreasing lower
temperature should be used.
6. Experimental setup
Description of setup
It consists of Following parts:-
Flat bottomed tube: The flat bottomed tube is about 3 cm in diameter and 12 cm high
and is fitted with a thermometer.
Air jacket: The tube is surrounded by the air jacket.
Cooling bath: The jacket is surrounded in turn by a cooling bath containing freezing
mixture. The freezing mixture can be crushed ice and salt or ice and CaCl2 or solid CO2 and
petrol, depending upon the cooling temperature required. A thermometer is inserted in the
cooling bath to determine the temperature.
7. Procedure
1. Clean and dry the lubricating test tube
2. Fill the oil up to the mark and fill the oil upto the mark and feed the tube with a cork with
thermometer.
3. Keep the tube in cooling jacket surrounded by freezing mixture.
4. The tube is taken out of the freezing mixture after every one degree fall in temperature and
inspect for the cloudiness.
5. If cloudiness appear note the temperature
24

6. Continue the cooling and take out the tube after every three degree fall of temperature to see
movement of oil.
Page

7. If the movement is there replace it immediately in the jar


8. Continue the test until no movement of oil is observed
9. When the test tube is held in a horizontal position for five seconds note down the temperature
and report the result.
8. Bill of Material: Cloud and pour point apparatus, Lubricating oil sample, Freezing mixture,
Thermometer, Cloud and pour point test tube etc.
9. Expectations
1. Experiment should be clearly performed according to temperature condition.
2. Maintenance of temperature should be proper with respect to outer environment.
3. There should be keen observation between cloud and pour point.
4. Reading obtained must follow temperature condition.
Students are expected to submit the following in their own handwriting and style:
1. Self assessment questions with reasoning.
2. Neat and clean labeled diagram.
3. Prepare value addition questions.
4. Result and justification of result should be in agreement with problem statement.
5. Readings should be noted down carefully for both observing points.

10. OBSERVATION TABLE:

S. No. Temperature (0C) Observation Inference


1
2
3
4
5
6

RESULT:
The cloud point of the given lubricant oil is _______and the pour point of the given
lubricating
oil is __________.

25
Page
ANILINE POINT APPARATUS

1. Aim: To determine Aniline Point of given lubricating oil by Aniline point Apparatus.
2. Objectives:
 What is Aniline point?
 Why we determine Aniline point.
 Significance of Aniline point determination.
 How it affects working of lubricating oil.
3. Outcomes:
 Able to know basic properties of lubricants
 Significance of Aniline point in engineering.
 Safeguards against deteoration.
 Able to apply basic property in applied mechanism
 Importance and use of different type of apparatus and their significance.

4. Theory with self-assessment questionnaire and problem enunciation:


Aniline point of oil is defined as the lowest temperature at which equal volumes of freshly distilled
aniline and oil are miscible. For the determination of aniline point equal volumes of sample and
aniline are taken in a test tube. The mixture is heated till a homogenous solution is obtained. The
tube is allowed to cool at uniform rate. The temperature at which the two phases separate out is
recorded as the aniline point. The separation of the two phase is indicated by the appearance of
cloudiness in the medium. High aniline point of a diesel fuel means low aromatic content and low
aromatic content means less knocking in diesel fuel.
Self assessment: 1
1. What do you mean by aniline point?
2. Define chemical nature of aniline?
3. Aniline point of lubricating oil should be?
4. Define significance of aniline point
5. How aniline point affect working of machinery
6. Is there any relation between aniline point and ignition quality of a diesel fuel?
Significance:
 Aniline point is a measure of aromatic content of the lubricating oil.
 A lubricating oil with low aniline point have a high aromatic content and will attack the rubber
seals used in the system this is because the aromatic compound have a tendency to dissolve
natural and certain types of synthetic rubbers.
 A higher aniline point means low percentage of hydrocarbon and hence is desirable.
 Thus aniline point used as an indication of possible deteoration of rubber sealings etc.
Self assessment: 2
7. Why we dry aniline before use?
8. Name dehydrating agent used to dry aniline.
9. Describe use of stirrer in aniline point apparatus.
10. What do you mean by a homogenous solution.
11. Why we use measuring cylinder instead of pipette to take aniline?
12. If lubricating oil have high percentage of hydrocarbon than what will be the aniline point?.
26

13. If lubricating oil have high percentage of aromatic compound than what will be the aniline
point?.
Page

5. Precautions:
1. No moisture should be adhering to the apparatus. It should be absolutely dry.
2. As aniline is highly toxic it should not be sucked into the pipette by mouth. A pipette
provided with rubber suction bulb should be used.
3. Precaution should be taken during stirring that no air bubbles should be formed.
6. Experimental setup
Description of setup
It consists of Following parts:-
Pyrex test tube: Pyrex test tube which is heat resistant and covers inner glass tube.
Glass test tube: The tube is used for observation and variation of aniline and oil.
Stirrer: It is used for stirring of both respective chemicals to make homogenous solution.
Heating burner: It is used to provide temperature.

7. Procedure
1. Clean and dry the aniline point apparatus
2. Take 5 ml of pure aniline and dry it over KOH pellet
3. Take 5ml of test oil and dry it by shaking with anhydrous Na2SO4
4. The aniline and the sample are transferred to test tube provided with a stirrer and a
thermometer.
5. This tube is inserted into an outer tube
6. The aniline and sample mixture is stirred to get a homogenous solution.
7. If not gets miscible than provide temperature and allow temperature to fall down at 1̊ C per
minute.
8. The temperature at which cloudiness or hazzyness appears is called aniline point.

8. Bill of Material: Aniline point apparatus ( test tube, thermometer, stirrer and heating bath).

9. Expectations
1. Experiment should be clearly performed according to temperature condition.
2. Maintenance of temperature should be proper with respect to outer environment.
3. There should be keen observation.
4. Reading obtained must follow temperature condition.
Students are expected to submit the following in their own handwriting and style:
1. Self assessment questions with reasoning.
2. Neat and clean labeled diagram.
3. Prepare value addition questions.
4. Result and justification of result should be in agreement with problem statement.
5. Readings should be noted down carefully for both observing points.

10. OBSERVATION TABLE:

S. No. Temperature (0C) Observation Inference


In decreasing order
1 Homogenous mixture of aniline
and oil
2
3
4
5
27

6 Oil and aniline separate out Aniline point


Page

RESULT:
The Aniline point of given lubricating oil is _______
STEAM EMULSION NUMBER APPARATUS

1. Aim: To determine Steam emulsion number (SEN) of given lubricating oil.


2. Objectives:
 What is steam emulsion number?
 Why we determine steam emulsion number
 Significance of SEN determination.
 How it affects working of lubricating oil.
3. Outcomes:
 Able to know basic properties of lubricants
 Significance of SEN in engineering.
 Safeguards against deteoration.
 Able to apply basic property in applied mechanism
 Importance and use of different type of apparatus and their significance.

4. Theory with self-assessment questionnaire and problem enunciation:


When water enters in an oil system turbulence is caused by high volume flow resulting in the
formation of emulsion. Some oil forms emulsion with water more easily than others. Due to the
formation of emulsion abrasion and wearing out of the lubricated parts of the machinery occurs.
Hence it is essential that the lubricating oil should form such an emulsion with water which breaks
off readily.SEN is defined as the time in seconds in which oil and water emulsion separates out in
distinct layer. The quicker the oil separates out from the emulsion the lower is the SEN and better
is the lubricating oil.
Self assessment: 1
1. What do you mean by Steam Emulsion Number?
2. Define term emulsification?
3. SEN of lubricating oil should be?
4. What are the drawbacks of forming emulsions why should it break off quickly?
5. Define significance to determine SEN.
Significance:
 To avoid corrosion of polished steel surface, it is important to check the speed of water and
oil separation.
 Formation of emulsion in most operations may be harmful as emulsification increases the
viscosity and consequently the coefficient of friction.
 Emulsion has a tendency to collect dirt, grit particles and other foreign matters which may
cause abrasion and wearing out of the lubricate parts to avoid corrosion of polished steel
surfaces, it is important to check the speed of water and oil separation.
 Steam emulsion number determines emulsion characteristics resulting from steam condensing
in oil.
 It is useful in defining the demulsibility of new oil.
 Exceptionally high values during service indicate foreign contamination of some component.

Self assessment: 2
6. Why emulsification increases viscosity?
28

7. Why emulsification causes abrasion and wear?


8. What do you mean by demulsification.
Page

9. Define homogenous solution


10. Why should good lubricating oil possess a low steam emulsion number?
5. Precautions:
1. The steaming rate should be so adjusted as to double the volume of the content of the tube
2. The end of the delivery tube should be cut at an acute angle and should dip in the test tube.
6. Experimental setup
Description of setup
The construction of apparatus is very simple. It consists of a steam generator which is a litre
round bottom flask heated from below with a burner . Test tube used as sample tube. The tube
is suspended in a emulsifying bath and another bath used as separating bath . Steam is led into
the sample by means of a delivery tube. As steam introduce in an oil sample a homogenous
solution is formed after certain heating and after that time noted down in seconds to determine
SEN.
7. Procedure
1. Clean and dry the test tube.
2. Take 20 ml of oil sample in a test tube.
3. Pass the steam through delivery tube into the oil. The steam jet violently agitates the oil and
forms emulsions.
4. Steam is admitted at such a rate as to raise the temperature of the emulsion to about 90ᵒC in
about 1 minute.
5. Continue the steaming till the volume of emulsion in the test tube becomes 40+3 ml
6. Remove the delivery tube and immediately start the stop watch to measure the time.
7. The time in which the emulsion breaks is reported as SEN of oil.

8. Bill of Material: SEN apparatus , oil, steam

9. Expectations
1. Experiment should be clearly performed according to temperature condition.
2. Maintenance of temperature should be proper with respect to outer environment.
3. There should be keen observation.
4. Reading obtained must follow temperature condition.
Students are expected to submit the following in their own handwriting and style:
1. Self assessment questions with reasoning.
2. Neat and clean labeled diagram.
3. Prepare value addition questions.
4. Result and justification of result should be in agreement with problem statement.
5. Readings should be noted down carefully for both observing points.

10. OBSERVATION TABLE:

S. No. Time (Seconds) Observation Inference


1 Emulsion of oil &
water
2
3
4
5
6 Oil and water SEN
emulsion separates
out distinct layer
29

RESULT:
Page

The SEN of given lubricating oil is _______


CONE PENETROMETER APPARATUS

1. Aim: To determine penetration number of grease.


2. Objectives:
 What is penetration number?
 Why we determine penetration number
 Significance of cone penetrometer determination
 How it affects working of grease.
3. Outcomes:
 Able to know basic properties of semisolid lubricants
 Significance of penetration number in engineering..
 Able to apply basic property in applied mechanism
 Importance and use of different type of apparatus and their significance.

4. Theory with self-assessment questionnaire and problem enunciation:


Grease is essentially a semi-solid combination of a thickening or gel agent soap or a mixture of
soaps and liquid lubricants. Greases give a higher coefficient of friction than lubricating oils.
Penetration number value: Penetration number with respect to lubricating grease is the depth in
tenth of an mm that a cone of standard dimensions penetrates vertically into the sample under test,
under prescribed condition of weight (150 gm), temperature (20ᵒC).

LGI consistency numbers


ASTM worked (60 strokes)
NLGI number penetration at 25 °C Appearance
tenths of a millimetre
000 445-475 fluid
00 400-430 semi-fluid
0 355-385 very soft
1 310-340 soft
2 265-295 "normal" grease
3 220-250 firm
4 175-205 very firm
5 130-160 hard
6 85-115 very hard

1. Common greases are in the range 1 through 3. Those with a NLGI No. of 000 to 1 are
used in low viscosity applications. Examples include enclosed gear drives operating at
low speeds and open gearing. Grades 0, 1 and 2 are used in highly loaded gearing. Grades
1 through 4 are often used in rolling contact bearings. Greases with a higher number are
firmer, tend to stay in place and are a good choice when leakage is a concern.
30

2. Greases are applied to mechanisms that can only be lubricated infrequently and where a
lubricating oil would not stay in position. They also act as sealants to prevent ingress of
Page

water and incompressible materials. Grease-lubricated bearings have


greater frictional characteristics due to their high viscosity.
3. Grease consistency depends on the type and amount of thickener used and the viscosity of
its base oil. Grease’s consistency is its resistance to deformation by an applied force. The
measure of consistency is called penetration. Penetration depends on whether the
consistency has been altered by handling or working. To measure penetration, a cone of
given weight is allowed to sink into a grease for five seconds at a standard temperature of
25°C (77°F).
4. The depth, in tenths of a millimeter, to which the cone sinks into the grease is the
penetration. A penetration of 100 would represent solid grease while a penetration of 450
would be semifluid.
“The NLGI consistency number (sometimes called “NLGI grade”) expresses a measure of
the relative hardness of a grease used for lubrication, as specified by the standard
classification of lubricating grease established by the National Lubricating Grease
Institute (NLGI)”.

Self assessment: 1
1. What do you mean by penetration number of grease?
2. Define term penetration number?
3. Define grease
4. Why grease is called semisolid lubricant and describes their applications.
5. Define significance to determine penetration number.
6. What do you mean by NLGI number?
7. What do you mean by grease consistency?
8. How greases are prepared?
Significance:
 Penetration value of grease is a measure of its degree of stiffness wheather it is hard or soft.
The hardness of grease may vary from that of a heavy viscous liquid to that of a stiff mass.
 The lower the penetration value the harder the grease, which means pumping of grease is
difficult and coefficient of friction is more.
 However grease can better withstand higher loads at lower speeds. A higher penetration
number means softer grease, lower resistance to flow, increased pumpability but unable to
withstand higher loads and more attention will have to be paid to prevent leakage.
 Measurement of penetration number of unworked ( not subjected to working of grease
worker) and worked ( subjected to working by grease worker) samples can be utilized to
access the consistency of a grease and also to study its gel fluid reversibility.
 It is also used as a control test for product uniformity and serves as a basis for dividing
greases into different grades. Greases are prepared by saponification of fat with alkali
followed by mixing hot lubricating oil.
Self assessment: 2
9. What do you mean by lower penetration value and higher penetration value?
10. A high penetration number is not suitable why?
11. What do you mean by unworked and worked grease?
12. Define applicability of penetration number
13. Why should a good lubricating oil possess a low steam emulsion number?
14. What do you mean by penetration number 100 and 450?
15. Define use of NLGI number.
5. Precautions:
1. For perfect positioning or the cone in contact with the grease surface a mirror should be
used to remove parallax.
2. As far as possible all air voids in the sample should be eliminated.
3. On pressing the push button the cone must have a free fall
31

4. Before taking subsequent reading the cone should be wiped perfectly clean and surface of
grease should be smoother.
Page

6. Experimental setup
Description of setup
It consist of following parts
Heavy base- Heavy base for sample bearings
Grease cup- Cup used for grease in order to check penetration.
Penetration cone- Used for penetration
Dial- Dial show reading in mm
Leveling screw- For movement of rod and it also bear push button for movement.
7. Procedure
1. Using spatula sample packed into grease cup.
2. The grease cup is now placed on the labeled table.
3. The standard cone is fixed with the holder shaft.
4. By pressing the push button the shaft is released then a stop watch is started.
5. The cone is allowed to penetrate for 5 seconds.
6. The dial rod is now pressed down until it is stopped by holder shaft.

8. Bill of Material: 150 gm weight, grease cup, standard cone, grease sample.
9. Expectations
1. Experiment should be clearly performed according to temperature condition.
2. Maintenance of temperature should be proper with respect to outer environment.
3. There should be keen observation .
4. Reading obtained must follow accuracy.
Students are expected to submit the following in their own handwriting and style:
1. Self assessment questions with reasoning.
2. Neat and clean labeled diagram.
3. Prepare value addition questions.
4. Result and justification of result should be in agreement with problem statement.
5. Readings should be noted down carefully for both observing points.

10. OBSERVATION TABLE:

S. No. Applied weight in gm Penetration in mm


1
2
3
4
5
6

Calculation: Average of three readings = (1+2+3)/3 X 1/10.

RESULT:
The penetration number is _______ mm.
32
Page
Water Analysis
Introduction: Water is one of the most important compounds for the existence of life.Water is always
used for drinking, sanitation, washing, irrigation, fire-fighting, cooling and in almost all industrial
work. But it also contains adulterations rendering it unsuitable without an application specific
treatment thereby we remove chemicals from the water not desired for a given application.

Sources of Water:
The two common sources of water are surface water and Ground water.
 Surface water occurs as rivers, streams, ponds, lakes, and wetlands.
 Ground water occurs in the pore spaces within rocks and alluvium, in fractures, and in
solution openings or conduits in areas underlain by soluble carbonate rocks such as limestone.

General applications of water:

• Potable water for consumption of living beings,


• General domestic washing of clothes, cleaning of toilets and floor,
• Medical treatment,
• Curing of structures in civil engineering
• In boilers
• Cooling and cleaning such as in Automobiles in battery, for cooling, in windscreen wiping etc.
• Cleaning of electronic circuit board process
• In numerous industrial processes.

Common impurities in natural water:


1. Physical impurities 2. Chemical impurities 3. Biological impurities

1. PHYSICAL IMPURITIES:
a. Colour: metallic substances like salts causecolour in water.
b. Turbidity: fine insoluble suspensions like clay, slit, and micro-organisms cause turbidity.
c. Taste: dissolved minerals in water produces taste.It can be bitter due to thepresence of Fe, Al,
Mn, Sulphates, lime. For ex. presence of sodium bicarbonate tastes like soap.
d. Odor: Odor in water repels its use for domestic as well as industrial purpose

2. CHEMICAL IMPURITIES:
a. Inorganic chemicals (Minerals) in the form of :
a. Cations: Ca+2, Mg+2, Na+, K+, Fe+2, Al+3, Zn+2, Cu+2, Mn+2
b. Anions: Cl-, SO-2, NO3-, HCO3-, F-, NO2-, SiO2
b. Organic chemicals: dyes, paints, petroleum products, pesticides, detergents, drugs textile
materials, and many other.
c. Acidity: industrial wastes like acid, mines,drainage, pickling liquors, presence of free CO2,
mineral acids, andweakly dissociated acids.
d. Gases: Most natural waters contains dissolved CO2, O2, NH3 gases, pollutant; nitrogen
content comes from urea and nitrogenous organic compounds, whichare partially converted
into NH3.
3. BIOLOGICAL IMPURITES:
Biological impurities such as Algae, pathogenic bacteria, fungi, viruses, pathogens, parasite-
33

worms, etc. the source of these contamination. These follow the discharge of domestic and
sewage wastes, excreta, etc.
Page

A. Micro-organisms: algae, fungi, viruses, etc.


B. Water bodies in water include
 Bacteria, organisms habituating in the bottom sludge, and
 Organisms and planktons developed at the water surfaces. These are inhibitated by worms
like flat worms, hair worms, tiny roundworms, oligochetes, etc.
CHARACTERISTICS OF WATER
As per the suggestion given by World Health Organization (WHO) & by Indian Council of Medical
Research (ICMR), the following are the desired characteristics of potable water.
1. Clear and colorless,Odorless.
2. It should be cool & pleasant to taste.
3. Free from harmful bacteria & suspended impurities.
4. Free from dissolved gases like CO2, H2S & poisonous minerals like lead, arsenic, manganese
etc.
5. Hardness < 500 ppm.
6. Chloride content < 250 ppm.
7. Fluoride content, 1.5 ppm.
8. Total dissolved solid < 500 ppm.
9. PH in the range of 6.5 to 8.5
BIS STANDARDS

S. Parameter BIS mg/L General & Health effect


N
1 Total dissolved Guideline
<2000 Undesirable taste; gastro intestinal irritations; corrosion or incrustation
o. solids value
2 PH 6.5-8.5 Affects mucous membrane; bitter taste; corrosion; affects aquatic life
3 Alkalinity <600 Boiled rice turns yellowish
4 Hardness <600 Poor lathering with soap; deterioration of the quality of clothes; scale forming;
skin irritation;
5 Calcium <200 Poor
boiledlathering
meat andand deterioration
food deterioratesquality of clothes; incrustation in pipes; scale
in quality
formation
6 Magnesium <100 Poor lathering and deterioration of clothes; with sulfate laxative
7 Iron <1 Poor or sometimes bitter taste, color and turbidity;staining of clothes materials;
iron bacteria causing slime
8 Manganese <0.3 Poor taste, color and turbidity; staining; black slime
9 Aluminum <0.2 Neurological disorders; Alzheimer's disease
10 Copper <1.5 Liver damage; mucosal irritation, renal damage anddepression; restricts growth
of aquatic plants
11 Zinc <15 Astringent taste; opalescence in water; gastro intestinalirritation; vomiting,
dehydration, abdominal pain,nausea and dizziness
12 Ammonia - Indicates pollution; growth of algae
13 Nitrite - Forms nitroso-amines which are carcinogenic
14 Nitrate <100 Blue baby disease (methemoglobineamia); algal growth
15 sulphate <400 taste affected; laxative affect,gastrointestinal irritation
16 chloride <1000 Bitter taste; corrosive
17 Fluoride mg/L
<1.5 Dental and skeletal fluorosis; non-skeletal
18 Phosphate mg/L
- Algal growth
19 Arsenic <0.05 Toxic; bio-accumulation; central nervous system affected; carcinogenic
20 Mercury <0.001 Highly toxic; causes 'minamata' disease-neurologicalimpairment and renal
disturbances; mutagenic
21 Cadmium <0.01 Highly toxic; causes 'itai-itai' disease-painful rheumaticcondition; cardio
34

vascular system affected;


22 Lead <0.05 gastrointestinal
Causes plumbism-tiredness,
upsets and hyper
lassitudes,
tensionabdominal discomfort, irritability,
Page

anaemia; bio-accumulation; impaired neurological and motor development, and


damage to kidneys
23 Chromium <0.05 Carcinogenic; ulcerations, respiratory problems and skin complaints
24 Pesticide <0.001 Affects central nervous system
25 Detergent - Undesirable foaming
ALKALINITY

Alkalinity: Alkalinity is a measure of the capacity of water to neutralize acids, alkaline compounds in
the water such as bicarbonates (HCO3-), carbonates (CO32-), and hydroxides (OH-) remove H+ ions
and lower the acidity of the water.Alkalinity is due to presence of soluble hydroxide (OH -), carbonate
(CO32-) & bicarbonate (HCO3) ions. These can be determined by titrimetry using standard acid (HCl
or H2SO4), phenolphthalein & methyl orange as indicators. Alkalinity is classified into two types
based upon the anion present in the water:

(i) Caustic alkalinity: due to (OH-) & (CO32-)


(ii)Temporary hardness: due to (HCO3-)
The possible combinations in which these ions can be present in water are:
1. OH- only
2. CO3- -only
3. HCO3- only
4. OH- & HCO3- together
5. CO3-- & HCO3- together

The other possibility i.e. OH & HCO3- together is ruled out due to the following reaction:
OH- + HCO3- H2O + CO32-

Due to the same reason all the three ions CO3-- & HCO3- & OH- cannot co-exist.
The determination is based on the following reactions
(i) (OH-) + (H+) H2O P
(ii) (CO32-) + (H+) (HCO3-) M
(iii) (HCO3-) + (H+) H2O + CO2

CALCULATION OF ALKALINITY OF WATER

Results of P & OH- CO32- HCO3- Nature of


M end point ppm ppm ppm alkalinity
P=0 O O M Only bicarbonate

P = 1/2 M O 2P O Only carbonate

P < 1/2 M O 2P M – 2P Bicarbonate &


carbonate
P > 1/2 M (2P – M) 2(M –P) O Hydroxide &
carbonate
P=M P or M O O Only hydroxide
35
Page
ALKALINITY TITRATION

1. Aim: To determine the alkalinity (type & extent) of a given water sample by acid –base titration
(neutralization titration) method.
2. Objectives:
 Explain the different characteristics of water.
 Estimate alkalinity of water and determine the type & extent of alkalinity present in water.
 To determine alkalinity of water by qualitative method
 Describe the reaction between alkalinity and certain cations present in water.
3. Outcomes:
 Students will able to know chemical analysis by titration
 Decide the tolerable limits of various compounds in water for a given application.
 Measurement of contaminations
 Conditioning/Processes to render the available water useful for an application.
4. Theory with self-assessment questionnaire and problem enunciation:
Determination of alkalinity due to different ions is based on the titration of the water
sample against a standard acid making selective use of indicators. The indicators used are –
phenolphthalein and methyl orange. The reactions taking place may be represented by the
following equations:

(i) (OH-) + (H+) H2O [P]


(ii) (CO32-) + (H+) (HCO3-) [M]
(iii) (HCO3-) + (H+) H2O + CO2

The volume of the acid used up to phenolphthalein end point corresponds to the reaction
(i)and (ii) i.e. complete neutralization of OH- ions and neutralization of CO3 - ions upto
HCO3 – stage
[Half neutralization of CO3- - ions].
The volume of the acid used up to methyl orange end point corresponds to the reaction
(i),(ii) & (iii)i.e. complete neutralization of OH- , CO3-- and HCO3- ions.
Thus from the respective volume of the acid used, the respective strengths of various ions
can be determined.
A known volume of the sample is titrated against a standard acid using phenolphthalein as
indicator and alkalinity is found out in terms of CaCO3 equivalents by using normality
equation. This alkalinity is called phenolphthalein alkalinity [P]. Similarly the sample is titrated
against a standard acid using methyl orange as indicator and alkalinity is calculated in
terms of CaCO3 equivalents. This alkalinity is called methyl orange alkalinity [ M ] or total
alkalinity of water sample.
From the measurement of phenolphthalein alkalinity and methyl orange alkalinity, it is
possible to calculate the magnitude of various forms of alkalinity present in water sample.

1. When P=0, alkalinity is due to HCO3- only.


2. When P= ½ M, only CO32- is present.
36

3. When P=M, only OH- is present.


Page

4. When P> ½ M OH- and CO32- are present.


5. When P< ½ M CO32- and HCO3- are present.
Self Assessment 1
1. What do you mean by titration?
2. Define end point.
3. What do you mean by alkalinity of solution?
4. Why OH‐ and HCO3‐ ions cannot exist together in water
5. What are the draw backs of using highly alkaline water?
6. What is caustic embrittlement and what are its drawbacks?
7. Describe values of P &M and correlate with types of ions present.
8. Why the alkalinity of irrigation water is determined?

Methyl orange indicator: Methyl orange is a pH indicator frequently used in titrations. In a


solution becoming less acidic, methyl orange moves from red to orange and finally to yellow with
the reverse occurring for a solution increasing in acidity. The entire colour change occurs in acidic
conditions.

Structure of methyl orange

Phenolphthalein indicator: Phenolphthalein is a chemical compound with the formulaC20H14O4


and is often written as "HIn" or "phph" in shorthand notation. Often used in titrations, it turns
colorless in acidic solutions and pink in basic solutions. If the concentration of indicator is
particularly strong, it can appear purple. In strongly basic solutions, phenolphthalein's pink color
undergoes a rather slow fading reaction and becomes completely colourless above 13.0 pH. The
molecule has four forms.

Structure of Phenolphthalein

The alkalinity of water is attributed to the presence of


37

(i) Caustic alkalinity( Due to OH‐ and CO32‐)


(ii) Temporary hardness ( Due to HCO3‐)
Page

Alkalinity is a measure of ability of water to neutralize the acids


Thymol Blue 1.2-2.8 1-2 drops 0.1% soln. in aq. red yellow
Pentamethoxy red 1.2-2.3 1 drop 0.1% soln. in 70% alc. red-violet colorless
Methyl yellow 2.9-4.0 1 drop 0.1% soln. in 90% alc. red yellow
Methyl orange 3.1-4.4 1 drop 0.1% aq. soln. red orange
Bromphenol blue 3.0-4.6 1 drop 0.1% aq. soln. yellow blue-violet
Bromcresol green 4.0-5.6 1 drop 0.1% aq. soln. yellow blue

The knowledge of alkalinity is essential due to following reasons:


 For calculating the amount of lime and soda required for water softening
 Highly alkaline water may lead to precipitates and form sludge in boiler tubes and pipes.
 In neutralization acidic solution
 To control the alkalinity of water being used for irrigation purposes.

The alkalinity of irrigation water is determined because the extent of alkalinity controls the growth
and development of different kind of plants, it also affects the fertilizers being used.

Self Assessment 2
9. How many types of alkalinity are there?
10. What do you mean by acid base titration
11. Describe other type of acid base indicator?
12. Define equivalent weight and molecular weight
13. What do you mean by normality of given solution
14. What do you mean by molarity of given solution.
15. What is the significance of alkalinity determination in water?
5. Precautions:
1. The beaker, pipette and the flask should be washed properly with distilled water.
2. Pipetting has to be accurate in order to avoid excess addition of the titrating agent.
3. The flask containing the indicator must be shaken well while acid is added to it.
4. The acid should be added dropwise.
5. Excess of indicator should not be used.
6. The flask into which acid is added dropwise should be removed as soon as the indicator
change color.
7. Readings should be taken avoiding the parallox error.
6. Procedure:
1. Pipette out 20 ml of water sample into a conical flask. Add 1‐2 drops of Phenolphthalein
indicator.
2. Rinse and fill the burette with N/10 HCl.
3. Titrate the water sample in conical flask with N/10 HCl till the pink color just
disappears.
4. Note down the reading and repeat to get same readings.
5. Again take 20 ml of water sample in conical flask and add methyl orange indicator
to it.
6. Titrate the water sample in conical flask with N/10 HCl till the yellow orange color
changes to orange red.
7. Note down the reading and repeat to get same readings.
38

7. Bill of Material: N/10 HCl, phenolphthalein and methyl orange indicators, Sample water.
Page

Burette, pipette, conical flask, beakers, funnel, and dropper


8. Expectations
1. Usually an air bubble is present in the nozzle of the burette; it must be removed before taking the
initial reading.
2. Their should not be any leakage from the burette during titration.
3. Keep your eye in level with the liquid surface while taking the burette reading or while reading
the pipette or measuring flask etc.
4. Always read lower meniscus in case of colorless solution and upper meniscus in case of colored
solutions.
5. Do not blow through the pipette to expel the last drop of solution from it.
6. Shaking of the titration flask should be continuous during adding the solution from the burette.
7. Use your index finger while pipetting the solution.
Students are expected to submit the following in their own handwriting and style:
1. Self assessment questions with reasoning.
2. Prepare value addition questions.
3. Result and justification of result should be in agreement with problem statement.
4. Readings should be noted down carefully after the complete process.

9. Observation Table:

S.No. Volume of Burette reading Phenolphthalein Methyl orange


water sample Initial [P] [M] end point [P] end point [M]
(ml)
1
2
3

CALCULATIONS:

39
Page

RESULT: The type of alkalinity present in water is___________


Extent of alkalinity:
DISSOLVED CHLORIDES

Chlorides are generally present in water in the form of NaCl and MgCl2 and may be due to leaching of
marine sedimentary deposits, pollution from sea water, industrial or domestic wastes etc. Their
concentration above 250mg/lit produce noticeable salty taste in water and thus objectional.
Further the presence of high quantity of chlorides in river or streams waters may indicte pollution of
water due to sewage and industrial wastes.
The presence of chlorides in the boiler water leads to problem like priming and foaming. Salts like
MgCl2 may undergo hydrolysis to form HCl leads to corrosion in boiler. Chorides in the form of
CaCl2 and MgCl2 causes hardness of water.
The chloride content of raw water should therefore regularly be tested.

ARGENTOMETRIC TITRATION

1. Aim: To determine dissolved chlorides in given water sample by Mohr’s method (


Argentometric titration)
2. Objectives:
 Explain the different characteristics of water.
 Estimate dissolved chlorides present in water.
 To determine dissolved chlorides of water by qualitative method
 Describe the various types of harmfull effects due to chloride ions.
3. Outcomes:
 Students will able to know chemical analysis by titration
 Decide the tolerable limits of various compounds in water for a given application.
 Measurement of contaminations
 Conditioning/Processes to render the available water useful for an application.
4. Theory with self-assessment questionnaire and problem enunciation:
Chlorides ions can be determined by titration of the water sample against a standard
solution of AgNO3 using potassium chromate as indicator (Argentometric titration) in a
neutral or faintly alkaline medium.
The solution of known strength is called the titrant while the solution which contains the
substance to be estimated is called titrate.
This determination is based on precipitation titration. When AgNO3 solution is added to the
water sample in presence of K2CrO4, The chlorides present in it precipitated as AgCl. As soon
as all the chlorides precipitated out even a drop of AgNO3 added in excess gives a red
precipitate of silver chromate. This indicates the end point.
AgNO3 + NaCl AgCl + NaNO3
AgNO3 + K2CrO4 Ag2CrO4 + 2KNO3
Main chloride contents are soil, rock, sewage and sea water.
There are three types of indicators
External indicator: Sometimes indicators is used outside as potassium fericyanide
Internal indicator: When indicator addedin solution
Self indicator: Solutions which change colour at end point are known as self indicator as
potassium permanganate.
Titration is classified into various types on the basis of the nature of chemical reaction
40

involved
Page

Acid base or neutralization titration


Redox titration
Precipitation titration
Complexometric titration
Iodometry titration
Iodimetry titration
Self assessment 1:
1. Define term titrate and titrant.
2. Is dissolved chrolides are harmfull? How it affects boilers.
3. Why it is called argentometric titration?
4. Why it is called Mohr’s method
5. Name indicator used in argentometric titration
6. What is the significance of chlorine estimation

The pH of the solution should be in between 7 to 8 because at higher pH Ag+ ions is precipitated
as AgOH
Ag+ + OH- AgOH
If the pH is lower than 7 to 8 then the chromate ion is converted to dichromate ion.
2CrO42- + 2H+ Cr2O72- + H2O
The required range can be achieved easily by adding a pinch of pure CaCO3. Excess CaCO3
being insoluble does
not interfere.
2H+ + CaCO3 Ca2+ + CO2 + H2O
Self assessment 2
7. How many types of titrations are there on the basis of chemical reactions?
8. How many types of indicator are there?
9. Why distilled water is always used in titration?
10. At what pH argentometric titration is performed? What happened if the pH is higher or
lower?
11. At the end point which colour appears?
12. What is the principle of argentometric titration.

5. Precautions:
1. The whoe apparatus should be washed with distilled water
2. The same amount of indicator must be added each time.
6. Procedure:
1. Pippete out 10 ml of distilled water in a conical flask and addone drop of K2CrO4 indicator.
2. Titrate it against N/50 AgNO3 solution till the brick red coour appear in the solution.
3. Note the reading ad repeat to get three concordant readings.

7. Bill of Material: N/50 AgNO3, K2CrO4 indicator, Sample water.Burette, pipette, conical
flask, beakers, funnel, and dropper
8. Expectations
1. Usually an air bubble is present in the nozzle of the burette; it must be removed before taking the
initial reading.
2. Their should not be any leakage from the burette during titration.
3. Keep your eye in level with the liquid surface while taking the burette reading or while reading
the pipette or measuring flask etc.
4. Always read lower meniscus in case of colorless solution and upper meniscus in case of colored
41

solutions.
5. Do not blow through the pipette to expel the last drop of solution from it.
Page

6. Shaking of the titration flask should be continuous during adding the solution from the burette.
7. Use your index finger while pipetting the solution.
Students are expected to submit the following in their own handwriting and style:
1. Self assessment questions with reasoning.
2. Prepare value addition questions.
3. Result and justification of result should be in agreement with problem statement.
4. Readings should be noted down carefully after the complete process.
9. Observation Table:

S.No. Volume of the Burette reading Volume of the


solution taken titrant used
in the flask (Final)
Initial Final

1
2
3

CALCULATIONS:

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RESULT: The chloride ion concentration in given water sample is___________


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