Chapter # 2

Literature Review
2.1) History of Brake Fluids
In the 1920's, when automobiles started switching from mechanical brakes
actuated by cables and levers to hydraulic brakes, the only material available for
the required flexible hoses was natural rubber. As a result, a hydraulic fluid
compatible with natural rubber was required for this application and a mixture of
castor oil and alcohol was found to meet this need. The use of this fluid enabled
the development of hydraulic brakes in the 1920's before synthetic rubbers
became available. However, it fixed this industry on the use of hydraulic fluids
based on glycols, glycol ethers, alcohols, poly-glycols and other related compounds
that can be used with elastomeric braking system components made of natural
rubber, styrene, butadiene, ethylene, propylene rubber, or poly-chloroprene. As a
result, brake fluids are completely different from any of the other fluids used in
automotive systems.
The first hydraulic system was devised in 1914 by American automotive
pioneer Frederick Duesenberg, and Lockheed Corporation co-founder Malcolm
Lougheed developed his own system in 1918.
Today's Lockheed, Girling, and silicone brake fluids are so vastly superior to
the old Girling "Green" and "Crimson", and Lockheed "Heavy Duty" fluids
originally. The most notable advances have been in raising boiling points,
improving compatibility with other brake fluids, reducing moisture absorption, and
reducing corrosion.

2.2) Brake System Fundamentals

The main function of brake fluid is to transmit the force applied to the brake
pedal to the brake pads and shoes. The foundation of any hydraulic system is
Pascals Law, which is generally given as in a fluid at rest in a closed container, a
pressure change in one part is transmitted without loss to every portion of the
fluid and to the walls of the container. To do this efficiently, brake fluids must be
non-compressible. In addition, they must also not boil at the highest operating
temperatures encountered, not thicken or freeze at cold temperatures, not corrode

or chemically react with any materials in the hydraulic system, and not decompose
or form sludge, gum, or varnish at any temperature. They must lubricate internal
moving parts, flow easily through small passages, have a long and stable shelf life,
and be compatible with other brake fluids.
When brakes are applied on a moving car, the kinetic energy of the vehicle in
motion is converted into heat. The faster the car is moving and the faster it is
stopped, the more heat is produced. Some of this heat soaks into the brake fluid.
In the late 1940s, brake fluid with a boiling point of 235F was considered
adequate. By about 1957, 302F was the lowest S.A.E. specification for a
minimum boiling point for cars with drum brakes.
Disc brakes presented new problems. In stopping faster (and often heavier)
cars more quickly, they generated even more heat which had to be dissipated.
Improvements in brake lining materials, brake drum and rotor design and
metallurgy have also had a similar effect. To handle these higher temperatures,
improvements had to be made in wheel cylinder and brake caliper seal design and
materials. The extra heat created a requirement for brake fluid that would not boil
at the new normal operating temperatures of vehicle brake systems. Brake fluids
must not be allowed to boil for two reasons. The first is simple: the brakes won't
work because the vapor bubbles formed in the boiling fluid are compressible, and
pressing on the brakes will compress the bubbles without exerting any pressure on
the brake pads or shoes. The second problem is more subtle, but equally serious
in the long term. When brake fluid boils, the physical and chemical properties will
be changed because some of the components will be affected. The brake fluid
contains chemicals that inhibit corrosion and oxidation, and these chemicals are
affected by very high temperatures. Brake fluid that has boiled will boil at a lower
temperature in the future.

2.3) Developments in Brake Fluids

The first brake fluids developed in 1920s were a mixture based on castor oil,
and the seals were made of leather. By the end of 1930s all U.S. automobiles have
rubber seals in the brake hydraulic systems.
In the U.S.A., ever-increasing use is being made of new brake fluid standards
introduced in 1973, FMVSS No. 116 (DOT-3 and DOT-4), which are aimed at

preventing the formation of vapor lock in brake systems: these standards have
introduced the quality index boiling point of wet fluid or boiling point of brake
fluid in working conditions. The standard J1703f, which was issued in 1975, is
only a little different from its predecessor, with only slight changes in the test
procedures.
Current brake fluids are based on polyoxyalkylene glycols and monoalkyl ethers
of these glycols, as these materials provide high point s and satisfactory lowtemperature properties. In order to eliminate the harmful effect of water, it has
been proposed that the brake fluids should include esters of boric acid with
alcohols or with alkylene glycol ethers.
After 40 years of research and development, a brake fluid that was acceptable
under extreme operating conditions was developed. This fluid achieved low water
pickup and good corrosion protection. The fluid also provides good lubrication
qualities and rubber compatibility. This was silicone brake fluid and has been
used in all military vehicles since the end of 1982.

Chapter # 3
Experimental Setup
3.1) Raw Materials
The raw materials needed for the production of Ethyl Benzoate which is a base
component for production of Hydraulic Brake Fluid on laboratory scale are as
follows,
1. Ethanol
2. Benzoic Acid
3. Sulfuric Acid (Concentrated)
4. Sodium Carbonate (Solution)
5. Ether (di-ethyl ether)

3.1.1) Ethanol
Ethanol, also known as ethyl alcohol, alcohol, Methylcarbinol, grain alcohol,
Ethyl hydroxide, Ethyl hydrate, Algrain, Anhydrol, Tecsol, is a volatile, flammable,
colorless liquid with the structural formula CH 3CH2OH, often abbreviated as
C2H5OH

or

C2H6O.

Ethanol

is

a psychoactive

drug and

is

one

of

the

oldest recreational drugs still used by humans. Ethanol can cause alcohol
intoxication when consumed. Best known as the type of alcohol found in alcoholic
beverages, it is also used in thermometers, as a solvent, and as a fuel. In common
usage, it is often referred to simply as alcohol or spirits.

3.1.1.1) Production of Ethanol

Ethanol is produced both as a petrochemical, through the hydration of
ethylene and, via biological processes, by fermenting sugars with yeast. The
economics of process depends on prevailing prices of petroleum and grain feed
stocks.
Ethanol for use as an industrial feedstock or solvent is made
from petrochemical feed

stocks,

primarily

by

the acid-catalyzed hydration

of

ethylene, represented by the chemical equation

C2H4 + H2O CH3CH2OH
The catalyst is most commonly phosphoric acid, adsorbed onto a porous
support such as silica gel or diatomaceous earth. This catalyst was first used for
large-scale ethanol production by the Shell Oil Company in 1947. The reaction is
carried out with an excess of high pressure steam at 300 C (572 F).
Ethanol for use in alcoholic beverages, and the vast majority of ethanol for
use as fuel, is produced by fermentation. When certain species of yeast metabolize
sugar in reduced-oxygen conditions they produce ethanol and carbon dioxide. The
chemical equations below summarize the conversion:
C6H12O6 2 CH3CH2OH + 2 CO2
C12H22O11 + H2O 4 CH3CH2OH + 4 CO2
Fermentation is the process of culturing yeast under favorable thermal
conditions to produce alcohol. This process is carried out at around 3540 C (95
104 F). Toxicity of ethanol to yeast limits the ethanol concentration obtainable by
brewing;
higher
concentrations,
therefore,
are
usually
obtained
by fortification or distillation.

3.1.1.2) Physical and Chemical Properties of

Ethanol

Properties

Sr. #

Appearance

Colorless

Density

0.789 g/cm3 (at 20C)

Flash Point

-5F

Water Solubility

Completely Soluble

Flammable Range (LELUEL)

3.3%19%

Flash Point

48 F

Ignition Temperature

793F

3
4

Melting Point

173 F

Boiling Point

173F

10

Vapor Density

1.49

11

Vapor Pressure

44 mmHg

3.1.2) Benzoic Acid

Benzoic Acid is also known as Dracylic acid, Benzeneformic acid,
Carboxybenzene, benzenecarboxylic acid, with formula C 7H6O2 (or C6H5COOH), is a
colorless crystalline solid and a simple aromatic carboxylic acid. The name is
derived from gum benzoin, which was for a long time the only source for benzoic
acid. Its salts are used as food preservatives and benzoic acid is an important
precursor

for

the

synthesis

of

many

other

organic

substances.

The salts and esters of benzoic acid are known as benzoates.

3.1.2.1) Production of Benzoic Acid

Benzoic acid is produced commercially by partial
oxidation of toluene with oxygen.
The
process
is
catalyzed
by cobalt or manganese naphthenates. The process uses cheap raw materials, and
proceeds in high yield.

U.S. production capacity is estimated to be 126,000 tonnes per year (139,000

tons), much of which is consumed domestically to prepare other industrial
chemicals.
Benzoic acid is cheap and readily available, so the laboratory synthesis of
benzoic acid is mainly practiced for its pedagogical value. It is a common
undergraduate preparation. Benzoic acid can be purified by re-crystallization from
water because of its high solubility in hot water and poor solubility in cold water.
The avoidance of organic solvents for the re-crystallization makes this experiment
particularly safe.

3.1.2.2) Physical and Chemical Properties of

Ethanol

Properties

Sr. #

Appearance

Odor

Density

colorless crystalline solid

Faint, pleasant odor

1.2659 g/cm3

Water Solubility

2.9 g/L

Vapor pressure

0.001 hPa

Flash Point

250.7 F

Auto ignition Temperature

1058 F

Melting Point

252.34 F

Boiling Point

480.6 F

10

Refractive index

1.539

11

Viscosity

1.26 mPa

3.1.3) Sulfuric Acid

Sulfuric acid is a strong mineral acid with the molecular formula H 2SO4. It is
soluble in water at all concentrations. When it is mixed with water, a very
exothermic reaction occurs and the energy released can be enough to heat the
mixture to boiling. Therefore, concentrated sulfuric acid must be diluted by adding
slowly to cold water while the mixture is stirred to dissipate the heat. Sulfuric acid
has many applications, and is one of the top products of the chemical industry.
Principal uses include lead-acid batteries for cars and other vehicles, ore
processing, fertilizer manufacturing, oil refining, wastewater processing, and
chemical synthesis. About 65% of sulfuric acid produced annually is used in the
production of agricultural fertilizers.

3.1.3.1) Production of Sulfuric Acid

Sulfuric acid is produced from sulfur, oxygen and water via the conventional
contact process.
Contact process:

In the first step, sulfur is burned to produce sulfur dioxide.

S (s) + O2 (g) SO2 (g)
This is then oxidized to sulfur trioxide using oxygen in the presence of
a vanadium (V) oxide catalyst. This reaction is reversible and the formation of the
sulfur trioxide is exothermic.
2 SO2 (g) + O2 (g)

2 SO3

The sulfur trioxide is absorbed into 9798% H2SO4 to form oleum (H2S2O7),
also known as fuming sulfuric acid. The oleum is then diluted with water to form
concentrated sulfuric acid.
H2SO4 (l) + SO3 (g) H2S2O7 (l)
H2S2O7 (l) + H2O (l) 2 H2SO4 (l)

Note that directly dissolving SO3 in water is not practical due to the
highly exothermic nature of the reaction between sulfur trioxide and water. The
reaction forms a corrosive aerosol that is very difficult to separate, instead of a
liquid.
SO3 (g) + H2O (l) H2SO4 (l)

3.1.3.2) Properties of Sulfuric Acid

Sr. #

Properties

Molecular formula

H2SO4

Molar mass

98.086 g/mol

Appearance

Clear, colorless, odorless liquid

Density

1.84 g/cm3, liquid

Melting point

10 C, 283 K, 50 F

Boiling point

337 C, 610 K, 639 F

Solubility in water

miscible

Acidity (pKa)

-31.99

Viscosity

26.7 cP (20 C)

10

Flash point

Non-flammable

3.1.4) Sodium Carbonate

Sodium carbonate (also known as washing soda, soda ash and soda crystals),
Na2CO3, is a sodium salt of carbonic acid (soluble in water). It most commonly
occurs as a crystalline hepta-hydrate, which readily effloresces to form a white
powder, the monohydrate. Pure sodium carbonate is a white, odorless powder that
absorbs moisture from the air, has an alkaline taste, and forms a strongly alkaline
water solution. Sodium carbonate is domestically well known for its everyday use
as a water softener.

3.1.4.1) Production of Sodium Carbonate

Mining:

Trona, trisodium hydrogendicarbonate dihydrate (Na3HCO3CO32H2O), is

mined in several areas of the US and provides nearly all the domestic consumption

of sodium carbonate. Large natural deposits found in 1938, such as the one
near Green River, Wyoming, have made mining more economical than industrial
production in North America. There are important reserves of Trona in Turkey; two
million tons of soda ash has been extracted from the reserves near Ankara. It is
also mined from some alkaline lakes such as Lake Magadi in Kenya by dredging.
Hot saline springs continuously replenish salt in the lake so that, provided the rate
of dredging is no greater than the replenishment rate, the source is fully
sustainable.
Leblanc process:

In 1791, the French chemist Nicolas Leblanc patented a process for

producing sodium carbonate from salt, sulfuric acid, limestone, and coal. First,
sea salt (sodium chloride) was boiled in sulfuric acid to yield sodium
sulfate and hydrogen chloride gas, according to the chemical equation
2 NaCl + H2SO4 Na2SO4 + 2 HCl
Next, the sodium sulfate was blended with crushed limestone (calcium
carbonate) and coal, and the mixture was burnt, producing calcium sulfide.
Na2SO4 + CaCO3 + 2 C Na2CO3 + 2 CO2 + CaS
The sodium carbonate was extracted from the ashes with water, and then
collected by allowing the water to evaporate.
The hydrochloric acid produced by the Leblanc process was a major source of
air pollution, and the calcium sulfide byproduct also presented waste disposal
issues.
Solvay process:

In 1861, the Belgian industrial chemist Ernest Solvay developed a method to

convert sodium chloride to sodium carbonate using ammonia. The Solvay
process centered around a large hollow tower. At the bottom, calcium carbonate
(limestone) was heated to release carbon dioxide:
CaCO3 CaO + CO2
At the top, a concentrated solution of sodium chloride and ammonia entered
the tower. As the carbon dioxide bubbled up through it, sodium bicarbonate
precipitated:
NaCl + NH3 + CO2 + H2O NaHCO3 + NH4Cl
The sodium bicarbonate was then converted to sodium carbonate by heating
it, releasing water and carbon dioxide:

2 NaHCO3 Na2CO3 + H2O + CO2

Meanwhile, the ammonia was regenerated from the ammonium chloride
byproduct by treating it with the lime (calcium hydroxide) left over from carbon
dioxide generation:
CaO + H2O Ca(OH)2
Ca(OH)2 + 2 NH4Cl CaCl2 + 2 NH3 + 2 H2O
Because the Solvay process recycles its ammonia, it consumes only brine and
limestone, and has calcium chloride as its only waste product. This made it
substantially more economical than the Leblanc process, and it soon came to
dominate world sodium carbonate production.
Hou's process:

Developed by Chinese chemist Hou Debang in 1930s. The earlier steam

reforming byproduct carbon dioxide was pumped through a saturated solution
of sodium chloride and ammonia to produce sodium bicarbonate via the following
reactions:
NH3 + CO2 + H2O NH4HCO3
NH4HCO3 + NaCl NH4Cl + NaHCO3
The sodium bicarbonate was collected as a precipitate due to its low solubility
and then heated to yield pure sodium carbonate similar to last step of the Solvay.

3.1.4.2) Properties of Sodium Carbonate

Properties

Sr. #

Molecular formula

Na2CO3

Molar mass

105.9885 g/mol (anhydrous)

124.00 g/mol (monohydrate)
286.14 g/mol (decahydrate)

Appearance

White solid, hygroscopic

Density

2.54 g/cm3 (anhydrous)

2.25 g/cm3 (monohydrate)
1.51 g/cm3 (heptahydrate)
1.46 g/cm3 (decahydrate)

Melting point

851 C (anhydrous)
100 C (monohydrate)
33.5 C (heptahydrate)
32 C (decahydrate)

Boiling point

1633 OC (anhydrous)

Solubility in water

71 g/L (0 C)
215 g/L (20 C)
455 g/L (100 C)

Basicity (pKb)

3.67

1.485 (anhydrous)
1.420 (monohydrate)
1.405 (decahydrate)

Refractive index

3.1.5) Di-ethyl Ether

Diethyl ether, also known as ethyl ether, sulfuric ether, simply ether,
or ethoxyethane,
is
an organic
compound in
the ether class
with
the
formula (C2H5)2O. It is a colorless, highly volatile flammable liquid. It is commonly
used as a solvent and was once used as a general anesthetic. It has narcotic
properties and has been known to cause temporary psychological addiction,
sometimes referred to as etheromania.

3.1.5.1) Production of Di-ethyl Ether

Most diethyl ether is produced as a byproduct of the vaporphase hydration of ethylene to
make ethanol.
This
process
uses
solidsupported phosphoric acid catalysts and can be adjusted to make more ether if the
need arises. Vapor-phase dehydration of ethanol over some alumina catalysts can
give diethyl ether yields of up to 95%.
Diethyl ether can be prepared both in laboratories and on an industrial scale
by

the

acid

ether

synthesis.[23] Ethanol is

mixed

with

strong

acid,

typically sulfuric acid, H2SO4. The acid dissociates in the aqueous environment
producing hydronium ions,

H3O+.

hydrogen

ion protonates the electronegative oxygen atom of the ethanol, giving the ethanol
molecule a positive charge:
CH3CH2OH + H3O+ CH3CH2OH2+ + H2O
A nucleophilic oxygen atom of unprotonated ethanol displaces a water
molecule from the protonated (electrophilic) ethanol molecule, producing water, a
hydrogen ion and diethyl ether.
CH3CH2OH2+ + CH3CH2OH H2O + H+ + CH3CH2OCH2CH3

This reaction must be carried out at temperatures lower than 150 C in order
to ensure that an elimination product (ethylene) is not a product of the reaction. At
higher temperatures, ethanol will dehydrate to form ethylene. The reaction to make
diethyl ether is reversible, so eventually an equilibrium between reactants and
products is achieved. Getting a good yield of ether requires that ether be distilled
out of the reaction mixture before it reverts to ethanol, taking advantage of Le
Chatelier's principle.

3.1.5.2) Properties of Di-ethyl Ether

Sr. #
1

Properties
Molecular formula

C4H10O

Molar mass

74.12 g mol1

Appearance

Colorless liquid

Density

0.7134 g/cm3, liquid

Melting point

116.3 C, 156.9 K, 177.3 F

Boiling point

34.6 C, 307.8 K, 94.3 F

Solubility in water

69 g/L (20 C)

Viscosity

0.224 cP (25 C)

Refractive index

1.353

10

Flash point

45 C

11

Auto ignition temperature

160 C

12

Explosive limits

1.9-48.0%

3.2) Experimental Work

3.2.1) Safety

Wear eye protection.

Protective gloves should be worn when handling acids and ether.
Proper ventilation should be provided in the laboratory.
Ether is highly flammable, keep away from ignition sources.
Concentrated sulfuric acid is very corrosive dense liquid, dehydrating

agent, add very slowly by continuously cooling the flask with water.
Do not empty the byproducts and unreacted chemicals into drains.

3.2.2) Preparation of Brake Fluid

3.2.2.1) Introduction
Brake fluids transmit the pressure on the brake pedal of a vehicle to the
brake shoes or pads, which rub on the wheels and slow them down. The fluids
must withstand high pressures without being compressed: air bubbles and vapors
prevent this. They need a high boiling point because heat is produced when the
brakes are applied. The fluid must also be chemically unreactive. It has been found
that certain esters meet these requirements best and industry uses esters from a
glycol and boric acid. An ester is formed when an alcohol and an acid react.

3.2.2.2) Preparation of an Ester

This experiment is to prepare an ester, ethyl benzoate, from ethanol and
benzoic acid, and then to purify it. The reaction involved is slow and needs heat to
get it working quickly. The reaction, which is reversible, i.e. it will go either way, is:
ACID + ALCOHOL

ESTER + WATER

To stop it reforming the acid and the alcohol, the water is removed with
concentrated sulphuric acid. To enable the reaction to be heated for a long time
and the liquid not to be lost, a condenser is placed over the boiling liquid so that
the vapors is cooled and returned to the flask.

Measured 100 cm3 of ethanol into a flask.

Slowly and carefully added 12 cm3 of concentrated sulphuric acid,
cooling the flask as this is being done by placing it under a running
tap.
Weighed 28 g of benzoic acid and added to the flask.
Arranged the apparatus as shown in Figure 1 and heated the flask over
gauze so that it boils gently.

Figure 1: Heating the mixture under reflux

Adjusted the flow of water in the condenser so that no vapors appear above

half way in the tube.

Heated the flask for an hour, and then left for five minutes with the water

running in the condenser to cool down the vapors.

Rearranged the equipment as shown in Figure 2, and then heated the water

gently.
Any ethanol that has not reacted with the benzoic acid will boil at 78 C and

was condensed and then collected.

Kept heating the water until there was no boiling in the flask: then all the
unchanged ethanol has been removed.

To remove any unchanged benzoic acid, added a solution of sodium

carbonate in water containing 8 g in 100cm3 until the liquid has a pH of

8 (test with universal indicator paper).

This changed the benzoic acid into sodium benzoate. The ethyl benzoate
was separated from this by using the fact that ethyl benzoate dissolves in

ether and sodium benzoate does not.

Poured the liquid into a separating funnel, added 40 cm3 of ether,
stoppered the funnel and shook for five minutes, removing the stopper

occasionally.
Left to settle, and then separated the two layers by pouring off the bottom
layer. Collected the two layers, running the ether layer into a clean, dry

flask. Added a further 10 cm3 of ether to the other liquid and repeated

the operation. Add this ether layer to the original ether in the flask.
To obtain the ethyl benzoate from this solution, distilled off the ether

using the equipment shown in Figure 2.

The ether boils well below the boiling point of water and is condensed and
collected in the tube. This enables the ether to be recollected so that it
can be used again. This recovery of the solvent is very important in
industry where solvents are used a lot and much money can be saved by

their recovery.
When all the ether had been boiled off, removed the beaker of water and
placed a tripod and gauze under the flask. Heated strongly with a Bunsen
and collected the liquid boiling at between 200 C and 215 C in a
container. This is the ethyl benzoate which can be used in the tests for
suitability as a brake fluid described in next section.

3.2.3) Tests on Brake Fluid

3.2.3.1) Introduction
To find if a liquid will work well as a brake fluid, its properties must be
tested. A brake fluid should:
a) have a high boiling point;
b) b) be tolerant to water mixing;
c) give suitable flow rates over a wide temperature change: the liquid must not
be syrupy (viscous) at low temperatures but must not get too thin at high
d)
e)
f)
g)
h)
i)

temperatures, otherwise it will not lubricate the brake shoes or act as a seal;
have no effect on rubber or plastic seals;
assist metals to resist corrosion;
be resistant to chemical change at high temperatures;
provide good lubrication for moving parts in the system;
mix with other brake fluids;
Not lose much volume by evaporation in working.
Industry needs to test all fluids used in braking systems to make sure that

they are up to standard in each of these respects. Below are some experiments
which were carried out in the laboratory to test whether the above properties are
present.

3.2.3.2) Finding the Boiling Point

Apparatus and chemicals required

Round-bottomed flask

 Liebig condenser
Thermometer
Bunsen burner
Stand and clamp
Anti-bumping granules
The boiling point of a liquid can be found in the laboratory by following way. The
method involves setting up the equipment as shown in Figure below.

Fig 3: Boiling Point Measurement

The best way to heat the flask is to use a variac-controlled heating mantle
that fits the flask. However, a Bunsen burner can be used, and the flame was
adjusted to give a constant boiling rate to the liquid. The liquid was heated until it
boil, with a condenser liquid flowing at a rate to keep the vapors condensing and
refluxing (the condensed liquid falls back into the original liquid). Adjusted the
heat so that the liquid boil gently and refluxes at a rate of two to four drops per
second. Left for five minutes to allow the condition to settle, and then taken the
temperature reading every 30 seconds for two minutes and the average result was
used.

3.2.3.3) Tolerance to water mixing

In normal use, brake fluids absorb small amounts of water which percolate in
from the surroundings through the brake hoses. This can affect the ability of the
fluid to operate at low temperatures as ice may form in the pipes, blocking the

system, and can lower the boiling point of the fluid, causing vapors to form in the
brakes. The effect of water on the boiling point of a typical brake fluid is shown in
the graph in figure.

Figure 4: Effect of moisture on boiling point of Brake Fluid

Apparatus and chemicals required

Measuring cylinder 250 cm3
Flask 250 cm3
Syringe 10cm3
Sample tube (2)
Beaker 250 cm3
Fluids to test
A sample of the test fluid can be contaminated with about 3 per cent water by measuring 200 ml
of the fluid in a measuring cylinder and pouring it into a flask, then adding 6 ml of water from a
syringe and shaking the flask for several minutes. This mixture can then be used for the following
tests. Filled a small sample tube with the mixture, sealed it and left it in a freezer overnight.
Tested the fluid for transparency and clearness by placing the tube over a
piece of graph paper and observing the lines through it. Examined the liquid for
traces of solid, turning it over several times. Another sample tube was taken and
filled with liquid and place it in a beaker of water at 60 C. Left for ten minutes to
allow the liquid to reach 60 C, then performed the same tests.

3.2.3.4) Viscosity
Apparatus and chemicals required

Glass tube (0.5m long, about 0.5 cm diameter)

Stopper to fit tube (2)

Water bath to fit tube
Fluids to test

A glass tube about 0.5 m long was taken, sealed at the bottom, and filled to
within 10 cm of the top with the fluid under test. Stoppered the top, then turned
the tube upside down and found the time needed for the air bubble to travel the
length of the tube. Left the tube in a freezer for half an hour, then repeated the
experiment. Placed the tube in a water bath at 100 C for ten minutes and then
repeated the experiment again. The quicker the bubble travels through the tube,
the lower the viscosity of the liquid. For a successful brake fluid, the viscosity
should remain constant over a large temperature range.
Another experiment that can be used to measure the flow of a fluid is to take
a glass tube 2 m long and about 2 cm internal diameter, fill it with the liquid
under test, then drop a ball bearing down the tube. Find the time it takes for the
ball bearing to reach the bottom of the tube. This can be tried at different
temperatures and using different liquids to compare their viscosity.

3.2.3.5) Effect on Rubber and Plastic Caps

Apparatus and chemicals required

Rubber sheet
Polypropene sheet
Cork borer
Micrometer screw gauge
Magnifying glass
Brake fluid
Isopropanol

Using a cork borer, cut two pieces of rubber sheet about 2 cm in diameter. Two
pieces of polypropene about the same size were taken. Measured the diameter of
each of the four pieces using a micrometer gauge. Placed one piece of rubber and
one piece of polypropene in the fluid under test and left for a week at room
temperature. After a week, removed the rubber and Polypropene from the fluid.
Held the pieces with tweezers and cleaned by rinsing in isopropanol, then dried in
warm air. Measured the diameter of the pieces under test within fifteen minutes of
removing them from the fluid. Using a magnifying glass, examined the surfaces for
blistering, pitting, or other signs of disintegration. Compared these samples with
the control samples which were not soaked in fluid. The fluid should not cause
corrosion of any sort or cause the material to expand by more than 5 per cent.

3.2.3.6) Effect on Metals

Apparatus and chemicals required

Samples of:

Aluminum
Brass
Copper
Cast iron
Tinned iron
Steel
Tin cutters
Emery cloth
Isopropanol
Beaker 250 cm3
Tweezers
Brake fluid
Access to balance

A brake fluid must not corrode the metals with which it comes into contact.
These metals may include cast iron, steel, tinned iron (tin plate), aluminum, brass,
and copper. To test this, strips of each metal were suspended in the fluid. The
strips were prepared by cutting pieces about 7 cm long and 1.8 cm across and
making a small hole near one end. The strips can be cleaned with emery cloth and
then were washed in isopropanol. Each strip was then handled only with tweezers.
Weighed each piece accurately and noted the weight. Assembled the metal strips
on a steel nail in the order tinned iron, steel, aluminum, cast iron, brass, and
copper, ensuring a gap at the top by bending the strips slightly. Washed again in
isopropanol to remove all dirt. Placed the metal strip assembly in a beaker and
poured sufficient liquid to cover by about 1 cm.
Left the assembly in the beaker in a water bath at about 80 C for a week.
Allowed the strips to cool in the fluid at room temperature for an hour. Using
tweezers removed the strips from the fluid; examine the strips for sediment and
shook them to remove any sediment which might be present. Cleaned each strip by
rubbing with a cloth soaked in isopropanol. Inspected each strip with a magnifying
glass for signs of pitting and corrosion. Weighed each strip and found the
differences in weight compared with the original weight. Found the weight loss per
unit surface area of the metal (remember there are two sides to each plate). This is
given by the formula:
Weight loss/unit surface area = Weight loss (mg)/Surface area (cm

3.2.3.7) Compatibility with other Brake Fluids

Apparatus and chemicals required

Measuring cylinder 100 cm3

Beaker 250 cm3
Sample tube
Brake fluid
Ester

Used a standard commercial brake fluid supplied in the lab for the following
test. Mixed 50 ml of the fluid under test with 50 ml of the commercial fluid in a
100 ml measuring cylinder. Mixed the fluid well in a beaker and examined for any
solid deposited and any layers forming. Poured into a sample tube, and then
inspected a piece of graph paper through it to test for deformation of the lines.
Placed the sample tube in the freezer for at least one hour, then repeated the test.
Placed in boiling water for fifteen minutes and carried out the test again. These
activities test the compatibility of the fluids at different temperatures.

3.2.3.8) Loss of Fluid by Evaporation

Apparatus and chemicals required

Petri dish
Fluid
Access to balance
It is important that a brake fluid maintains its volume under working conditions or an air lock
may develop, reducing the efficiency of the system and making the brakes 'spongy'. The amount of
evaporation in a closed system can be found by weighing an empty glass Petri dish with its lid on,
adding 25 ml of fluid from a measuring cylinder and then weighing again. The weight of fluid in the
dish can then be calculated. Placed the dish (with the lid on) in a ventilated oven at 100 C for two
days, then remove and left to cool at room temperature and weighed the dish again. Found the loss of
weight of the fluid and expressed it as a percentage of the original. This can be repeated for each
fluid.
% loss of weight = loose of weight / original weight

3.2.3.9) Lubricant
The lubricant properties of a fluid are related to its viscosity. If the fluid is too
thin, it runs off too easily; if it is too viscous, it offers resistance to movement and
also lessens its ability not to corrode the metals involved in the movement.

3.2.3.9) pH Value

It is important that a brake fluid should not produce an acid reaction with
the materials with which it comes into contact. The acceptable range for the pH of
a brake fluid is between 7 and 11.5.
To find the pH of the fluids under test, mixed 25 ml with 25 ml of a mixture
of 80 per cent ethanol and 20 per cent water, which had been neutralized to a pH
of 7. Determined the pH of the resulting solution by using universal indicator
solution or a pH meter with a calibrated electrode.

Chapter # 4
Results and Discussions
4.1) Table of Results
Test no.

Property

Sample

Guard
DOT 3

Dry Boiling
Point
Wet Boiling
Point
Specific
Gravity
Viscosity

170 oC

180 oC

122 oC

140 oC

0.9889

1.0841

4.54
Kg/mSec
No
Significant
Effect
No
Significant
Effect

9.5
Kg/mSec

2
3
4
5

Effect on
Rubber

Effect on
Copper

4.2) Discussins on Results

4.2.1) Boiling Point:

No Effect
No Effect

The dry boiling point of sample product produced is 170 oC. While the
boiling point of Guard DOT 3 is 180 OC. Hence our product has value of dry
boiling point much closer to the commercial product, although this small
difference is due to absence of additives.
Same is the case with wet boiling point.

4.2.2) Specific Gravity:

The specific gravity of sample product produced is 0.9889. while the specific
gravity of Guard DOT 3 is 1.0841. This shows that our product has almost
same value of specific gravity as that of commercial product.

4.2.3) Viscosity:

The viscosity of sample product produced is 4.54 Kg/m Sec. while the viscosity
of Guard DOT 3 is 9.50 Kg/m Sec. This difference in values of viscosities is due
to the fact that many additives are added in commercial product to improve
viscosity, while those additives are not added in our sample product.
The additives which are commonly used to improve properties of Brake Fluids
are:
1.
2.
3.
4.
5.
6.
7.
8.
9.

Tributyl phosphate,
Benzotriazole
Tolytriazole
Triethanol amine
Cyclohexyl amine
Dibutyl amine
Dibutylhydroxy toluene
Bisphenol A
3-diethanol aminopropyl Silane

4.2.4) Effect on Rubber:

There was no significant effect of sample product on rubber, as no swelling of
rubber was occurred on keeping rubber dipped in sample product for five days.
This indicates that our product is appropriate to be used against rubber.

4.2.5) Effect on Copper:

There was no significant corrosion effect of sample product on copper, as copper

strip was not corroded on keeping dipped in sample product for seven days. This
indicates that our product is appropriate to be used against copper tubes.