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CHEMISTRY LABORATORY MANUAL
(Common to Production / Mechanical – G1 Branches)
Course code 15P212 / 15M212
Course title CHEMISTRY LAB – II
NAME
ROLL NO
BRANCH PRODUCTION / MECH-G1 ENGINEERING
DEPARTMENT OF CHEMISTRY
PSG COLLEGE OF TECHNOLOGY

COIMBATORE- 641004.
CHEM LAB-II
Dr. SENTHILKUMAAR/CHEM PROD/MECH-G1

CHEM LAB-II
PSG COLLEGE OF TECHNOLOGY

COIMBATORE – 641004
LABORATORY MANUAL/RECORD
NAME
ROLL NO
BRANCH PRODUCTION / MECH-G1 ENGINEERING
CERTIFIED BONAFIDE RECORD OF WORK DONE BY
Mr / Miss
Date Signature of the faculty

(Dr. S. SENTHILKUMAAR)

CHEM LAB-II

CHEM LAB-II
TABLE OF CONTENTS
SEMESTER II
S.No Name of the Experiments Page

No.
A Determination of alkalinity and TDS of water.
1
Determination of acid value, saponification value and iodine number
B
of oils.
Electroplating of Nickel & Copper, and determination of cathodic

2
efficiency.
Determination of Redwood / Saybolt numbers and kinematic viscosity

A
of lubricating oils.
3
Proximate analysis of coal – determination of moisture, volatile
B
matter, ash and fixed carbon.
A Determination of efficiency of corrosion inhibitor.

4
B Determination of flash and fire point, cloud and pour point of oil.

CHEM LAB-II
GENERAL RULES OF LABORATORY SAFETY
1. Avoid keeping mobile phones during the laboratory hours.
2. Keep your belongings on the shelves provided and do not place bags or books on
the experiment tables.
3. The chemicals used in this laboratory are likely to be corrosive and/or toxic. Avoid
skin contact with any of these chemicals. It contact does occur; copiously wash the
area of contact with water.
4. Do not perform any unauthorized experiments.
5. Students at this level must not work alone in this laboratory.
6. Adequate foot covering is required at all times. Do not wear sandals. Do not enter
into the laboratory with bare feet.
7. Cold and hot objects often look the same. Remember always to exercise caution
when picking up laboratory glassware and tools.
8. Always notify the instructor in case of an injury.
9. As for the disposal of waste chemicals, when in doubt ask the instructor.
10. If you spill any reagents, clean them up immediately, if necessary rinse well with
water.
11. Keep your desk and reagent table clean and tidy at all times. After completing the
experiment, clean the apparatus used and the experimental place. Return the
reagent bottle to the lab assistants.
12. Dispose the solid waste in waste baskets. Do notput them in the sink.
13. If you break any glassware, immediately inform the lab assistants.

CHEM LAB-II
INDEX
For CA # 1.
Marks obtained Sign.
Expt. of the
Date Title of the Experiment Pre-lab
No. Observation
test faculty
(15)
(10)
1.
2.
Average = (1 + 2) / 2

CHEM LAB-II
GENERAL INSTRUCTIONS
1. Laboratory manual is considered as a proof of the laboratory work you have done.
Keep it neat and all pages intact.
2. While in laboratory, you should know what you are doing and why you are doing so.
In order to avoid unnecessary repetition of the experiments and loss of time, proper
preparation before starting the experiment is imperative.
3. Read the principle and experimental procedure of assigned experiment before

coming to the lab session.
4. Plan the sequence of steps of your experiment in such a way that it could be
completed within the stipulated time.
5. Experiment number and date should be entered at the beginning of every

experiment.
6. All entries must be made directly with a non-erasable ink/ball pen.
7. Under no circumstances should any pages be removed from the record notebook.
8. Do not use correction fluid, liquid paper, white-out or any product that covers up
original entries. Do not over write the readings in the laboratory manual.
9. Plan the organization of the data in your laboratory manual.
10. Write all observations/readings only in the laboratory manual.
11. All laboratory manual entries must be signed by your course instructor before
leaving from your laboratory after completion of the experiment.

CHEM LAB-II
For CA # 2.
Marks obtained Sign.
Expt. of the
Date Title of the Experiment Pre-lab
No. Observation
test faculty
(15)
(10)
1.
2.
Average = (1 + 2) / 2

CHEM LAB-II

CHEM LAB-II
Expt. A Determination of alkalinity and TDS of water.

No.
Date B Determination of acid value, saponification
value and iodine number of oils.
A. Determination of alkalinity and TDS of water.
AIM: To estimate the different types and amounts of alkalinity and total dissolved solid
content in water.
THEORY
The alkalinity of a water sample is a measure of its capacity to neutralize acids.

Alkalinity of water is due to the presence of basic constituents like carbonates (Na2CO3,
K2CO3), bicarbonates [NaHCO3, KHCO3, Ca(HCO3)2 and Mg(HCO3)2]and hydroxides
[NaOH, KOH].
Alkalinity reveals the buffering capacity of water and reflects how much acid is
required to change the pH. While pH measures the strength of an acid or base, alkalinity
indicates a solution’s power to react with an acid and "buffer" its pH. The alkalinity is
equal to the stoichiometric sum of the bases in solution.
The main sources of natural alkalinity are rocks, which contain carbonate,
bicarbonate, and hydroxide compounds. Limestone is rich in carbonates, so waters
flowing through limestone regions generally possess high alkalinity. Conversely, granites
do not have minerals and do not contribute to alkalinity. Therefore, waters flowing through
areas rich in granite have low alkalinity and poor buffering capacity.
Alkalinity is important for fish and other aquatic life because it protects or buffers
against pH changes and makes water less vulnerable to acid rain. Too much of alkalinity
imparts an unpleasant soda taste in water. Also, when in contact with the body, serious
dryness might occur on the skin because alkaline water tends to remove the oils present
in the human skin.
Significance of Alkalinity:
Neither alkalinity nor acidity, have any known adverse health effects. Nonetheless,
knowledge of these parameters are important because:
Dr. SENTHILKUMAAR/CHEM 1
PROD/MECH-G1
CHEM LAB-II
(1) The alkalinity of a body of water provides information about how sensitive that water
body will be to acid inputs such as acid rain and discharge of industrial effluents.
(2) Turbidity is frequently removed from drinking water by coagulation and flocculation.
This process releases H+ into the water. Alkalinity must be present in excess of that
destroyed by the H+ released for effective and complete coagulation to occur.
(3) Hard waters are frequently softened by precipitation methods. The alkalinity of the
water must be known in order to calculate the lime (Ca(OH)2) and soda ash (Na2CO3)
requirements for precipitation.
(4) The alkalinity is useful in estimating the Langelier saturation index (LSI). The LSI is
useful in determining whether the water is corrosive or has the ability to form scales of
CaCO3 in the inner wallsof plumbing.
- 2-
(5) Bicarbonate (HCO3 ) and carbonate (CO3 ) may complex with other elements and
compounds, altering their toxicity, transport, and fate in the environment.
(6) Municipal authorities usually prohibit the discharge of wastes containing caustic
alkalinity to sewers. Alkalinity as well as pH is an important factor in determining the
amenability of wastewaters to biological treatment.
(7) In boilers, carbon dioxide is insoluble in boiling water and so it is removed with the
steam. This causes an increase in pH and a shift in alkalinity forms from bicarbonate
to carbonate and from carbonate to hydroxide. This leads to increase in pH reaching
11, which may cause caustic embrittlement in the boiler material.
2HCO3¯  CO3 2¯ + H2O + CO2
2¯ ¯
CO3 + H2O 2OH + CO2
Estimation of alkalinity:
Alkalinity of water can be estimated by titrating against hydrochloric acid in successive
stages using phenolphthalein and methyl orange as indicators. Phenolphthalein end point
[P] indicates only the neutralization of hydroxyl ion and half of the carbonate ions.
1. OH- + H+ → H2O
2. CO3- + H+ → HCO3-
The bicarbonate ion cannot ionize phenolphthalein and hence does not produce its
characteristic color. Methyl orange end point [M] indicates complete neutralization of
bicarbonates, carbonates and hydroxyl ions
1. OH- + H+ → H2O
- + -
2. CO3 + H → HCO3
- +
3. HCO3 + H → H2O + CO2↑
Hydroxide and bicarbonate will not exist together since they will react with each
other.
- - 2-
OH + HCO3 → H2O + CO 3
Dr. SENTHILKUMAAR/CHEM 2 PROD/MECH-G1

CHEM LAB-II
The following table summarizes the interpretation of the phenolphthalein and methyl
orange alkalinities.
Finding the different alkalinities using [P] and [M] titre values
Alkalinity causing ions

Results of [P] and [M]
S.No.
Value from titration II OH- CO3 2- HCO3-
1. [P]=0 0 0 [M]
2. [P]= [M] [P] or [M] 0 0
3. [P]= ½ [M] 0 2[P] or [M] 0
4. [P] > ½ [M] 2[P] - [M] 2[M] - 2[P] 0
5. [P] < ½ [M] 0 2[P] [M] - 2[P]

CHEM LAB-II
Calculation
Titration I: Standardization of hydrochloric acid
Standard sodium carbonate Vs hydrochloric acid
Burette solution : Hydrochloric acid

Pipette solution : Standard sodium carbonate
Indicator : Methyl orange
Endpoint : Golden yellow to orange red
Volume of sodium Burette readings (ml)

Volume of hydrochloric
S.No. carbonate
Initial Final acid consumed (ml)
(ml)
Concordant value = ml
Calculation:
Volume of sodium carbonate solution V1 = ml
Normality of sodium carbonate solution N1 = N
Volume of hydrochloric acid solution V2 = ml
Normality of hydrochloric acid solution N2 = V 1 N1 / V 2
= N

CHEM LAB-II
PROCEDURE:
TITRATION I: STANDARDIZATION OF HYDROCHLORIC ACID
Exactly 20 ml of standard sodium carbonate solution is pipetted out into a clean

conical flask. A drop of methyl orange indicator is added to it, which gives a golden yellow
colour to the solution. It is titrated against hydrochloric acid taken in the burette. At the
end point, the golden yellow colour of the solution changes to orange red. The titrations
are repeated till concordant values are obtained. From the concordant value, the
normality of hydrochloric acid is calculated.
TITRATION II: ESTIMATION OF ALKALINITY
Exactly 20 ml of the alkaline water sample is pipetted out into a clean conical flask,
to which a drop of phenolphthalein indicator is added. It is titrated against the hydrochloric
acid taken in the burette. The end point of the titration is the disappearance of pink colour.
This titre value corresponds to the phenolphthalein end point [P]. Two drops of methyl
orange is added to the same solution and the titration is continued (without refilling the
burette). At the end point, the golden yellow colour of the solution changes to orange red.
This total titre value corresponds to methyl orange end point [M]. The titrations are
repeated till the concordant values are obtained. The alkalinities are expressed in terms
of calcium carbonate equivalents.
Equivalent weight of CaCO3 is 50 g
Equivalent weight of Na2CO3 is 53.g

CHEM LAB-II
Titration II: Estimation of alkalinity in water

Standardized HClVs alkaline water sample
Burette solution : Hydrochloric acid
Pipette solution : Alkaline water sample
Indicators : Phenolphthalein / Methyl orange
Endpoint : Disappearance of pink colour / Golden yellow to orange red
Burette readings(ml)
Volume of Volume of
S.No. alkaline water Final hydrochloricacid (ml)
sample(ml) Initial
P M P M
Concordant value (i). P = ml
(ii). M = ml
Calculation:
(i) Phenolphthalein alkalinity
Volume of hydrochloric acid consumed for
phenolphthalein end point V1 = ml
Normality of hydrochloric acid solution N1 = N
Volume of alkaline water sample solution V2 = ml
Normality of alkaline water sample solution N2 = V1N1 / V2
= N
Phenolphthalein alkalinity
(in term of CaCO3Equivalents) = N x 50 x 1000
= ppm

CHEM LAB-II
DETERMINATION OF TOTAL DISSOLVED SOLIDS (TDS):
Dissolved solids are mainly composed of chlorides, nitrates, sulphates, phosphates

of Na, K, Ca, Mg, Fe, Mn etc. The amount of dissolved salts can be found out by the
evaporating the filtered water followed by the weighing the residue.
A clean and dry beaker is weighed (w1). Exactly 20 ml of the filtered water sample is
transferred into the beaker and evaporated to dryness. The weight of the beaker with the
residue is noted (w2). From the difference in weight, the TDS is calculated.
REVIEW QUESTIONS:
1. pH buffering action of water is very much needed for the aquatic life. Otherwise
what would happen?
2. Hydroxide and bicarbonate does not exist together in a solution. Why?
3. What are the various ill effects of highly alkaline water?
4. What do you mean by calcium carbonate equivalent?
5. Justify the conditions involved in the estimations of different alkalinity causing ions
with relevant chemical equations.
6. Granite rocks do not cause alkalinity to water. Give reasons.
7. State the Beer- Lambert's law.
8. What is the permissible limit for TDS in drinking water?
9. What is the reason for the alkalinity of ground water?

CHEM LAB-II
(ii) Methyl orange alkalinity
Volume of hydrochloric acid for methyl orange end point V1 = ml

Normality of hydrochloric acid solution N1 = N
Volume of alkaline water sample solution V2 =ml
Normality of alkaline water sample solution N2 = V1N1/V2
= N
Methyl orange alkalinity
(in term of CaCO3Equivalents) = N x 50 x 1000
= ppm
Calculation for TDS:
Volume of water = _ mL
Weight of the empty beaker (W 1) = g
Weight of the beaker + residue (W 2) = g
Weight of the residue (W 2 - W 1) = g
= mg
Total dissolved solids in a 1litre of water sample = (W 2 - W 1) in mg X 1000
Volume of water taken
= ppm

CHEM LAB-II
B. Determination of acid value, saponification value and iodine

number of oils.
Fats and oils are the most abundant lipids in nature. They provide energy for living
organisms, insulate body organs, and transport fat-soluble vitamins through the blood.
Structures of Fats and Oils
Fats and oils are called triglycerides (or triacylcylgerols) because they are esters
composed of three fatty acid units joined to glycerol, a trihydroxy alcohol:
If all three OH groups on the glycerol molecule are esterified with the same fatty
acid, the resulting ester is called a simple triglyceride. Although simple triglycerides have
been synthesized in the laboratory, they rarely occur in nature. Instead, a typical
triglyceride obtained from naturally occurring fats and oils contains two or three different
fatty acid components and is thus termed a mixed triglyceride.
A triglyceride is called a fat if it is a solid at 25°C; it is called an oil if it is a liquid at

that temperature. These differences in melting points reflect differences in the degree of
unsaturation and number of carbon atoms in the constituent fatty acids. Triglycerides
obtained from animal sources are usually solids, while those of plant origin are generally
oils. Therefore, we commonly speak of animal fats and vegetable oils.
Terms such as saturated fat or unsaturated oil are often used to describe the fats
or oils obtained from foods. Saturated fats contain a high proportion of saturated fatty
acids, while unsaturated oils contain a high proportion of unsaturated fatty acids. The high
consumption of saturated fats is a factor, along with the high consumption of cholesterol,
in increased risks of heart disease.
Physical Properties of Fats and Oils
Pure fats and oils are colorless, odorless, and tasteless. The characteristic colors,
odors, and flavors that we associate with some of them are imparted by foreign
substances that are lipid soluble and have been absorbed by these lipids. For example,
the yellow color of butter is due to the presence of the pigment carotene; the taste of
butter comes from two compounds—diacetyl and 3-hydroxy-2-butanone—produced by
bacteria in the ripening cream from which the butter is made.
Fats and oils are lighter than water, having densities of about 0.8 g/cm 3. They are
poor conductors of heat and electricity and therefore serve as excellent insulators for the
body, slowing the loss of heat through the skin.
Chemical Reactions of Fats and Oils
Fats and oils can participate in a variety of chemical reactions—for example,

because triglycerides are esters, they can be hydrolyzed in the presence of an acid, a
base, or specific enzymes known as lipases. The hydrolysis of fats and oils in the
presence of a base is used to make soap and is called saponification. Today most soaps

CHEM LAB-II
Calculation:
ACID VALUE:
Weight of oil sample taken (w) =
Normality of KOH used (N) =
Volume of N normal KOH consumed

in the titration with oil sample (V) =
1000 ml of 1 N KOH ≡ 56 g of KOH
Therefore, V ml of N normal KOH ≡ 56 g
= g of KOH (let it be A)
Acid value, ie.the number of mg of KOH
required to neutralize 1 g of the oil =
SAPONIFICATION NUMBER:
Weight of oil sample taken (w) =
Normality of acid used (N) =
Volume of N normal acid consumed
in the titration with oil sample V1 =

CHEM LAB-II
are prepared through the hydrolysis of triglycerides (often from tallow, coconut oil,
or both) using water under high pressure and temperature. Sodium carbonate or sodium
hydroxide is then used to convert the fatty acids to their sodium salts (soap molecules):
The double bonds in fats and oils can undergo hydrogenation and also oxidation.
The hydrogenation of vegetable oils to produce semisolid fats is an important process in
the food industry.
In commercial processes, the number of double bonds that are hydrogenated is
carefully controlled to produce fats with the desired consistency (soft and pliable).
Inexpensive and abundant vegetable oils (canola, corn, soybean) are thus transformed
into margarine and cooking fats.
Fats and oils that are in contact with moist air at room temperature eventually
undergo oxidation and hydrolysis reactions that cause them to turn rancid, acquiring a
characteristic disagreeable odor. One cause of the odor is the release of volatile fatty
acids by hydrolysis of the ester bonds. Butter, for example, releases foul-smelling butyric,
caprylic, and capric acids. Microorganisms present in the air furnish lipases that catalyze
this process. Hydrolytic rancidity can easily be prevented by covering the fat or oil and
keeping it in a refrigerator.
Another cause of volatile, odorous compounds is the oxidation of the unsaturated
fatty acid components, particularly the readily oxidized structural unit
in polyunsaturated fatty acids, such as linoleic and linolenic acids. One particularly
offensive product, formed by the oxidative cleavage of both double bonds in this unit, is a
compound called malonaldehyde.
Rancidity is a major concern of the food industry, which is why food chemists are
always seeking new and better antioxidants, substances added in very small amounts
(0.001%–0.01%) to prevent oxidation and thus suppress rancidity. Antioxidants are
compounds whose affinity for oxygen is greater than that of the lipids in the food; thus
they function by preferentially depleting the supply of oxygen absorbed into the product.
Because vitamin E has antioxidant properties, it helps reduce damage to lipids in the
body, particularly to unsaturated fatty acids found in cell membrane lipids.
The acid value of oil is defined as the number of milligrams of potassium
hydroxide required to neutralize the free acid present in 1g of oil sample. An increment in
the amount of FFA in a sample of oil or fat indicates hydrolysis of triglycerides. Such
reaction occurs by the action of lipase enzyme and it is an indicator of inadequate
processing and storage conditions.
The saponification number of oil is the number of milligrams of potassium

hydroxide required to saponify one gram of the oil. The vegetable or animal oils are
esters of higher fatty acids and they react with KOH to form the potassium salts of fatty
acids. In this, a known weight of the sample is allowed to react with an excess of
standardized KOH solution and the alkali consumed in the saponification is estimated by
a back titration with a standardized acid solution.
Iodine value or iodine number is defined as the number of grams of iodine

consumed by 100g of the oil. Iodine adds to the unsaturated functional groups present in
the oil sample. In this, a known weight of the sample is allowed to react with an excess of
standardized iodine solution and the iodine consumed by the oil is estimated by a back
titration with a standardized sodium thiosulphate solution.

CHEM LAB-II
Volume of N normal acid consumed
in the blank titration V2 = ml
1000 ml of 1 N HCl (1 equivalent) reacts with 56 g (1 equivalent) of KOH
Therefore, V2 – V1 ml of N normal HCl reacts with 56 g
= g of KOH (let it be S)
Saponification number, ie.the number of mg
of KOH required to saponify 1 g of the oil =
IODINE VALUE:
Weight of oil sample taken (w) = g
Normality of thio used (N) = N
Volume of N normal thio consumed
in the titration with oil sample V1 = ml
Volume of N normal thio consumed
in the blank titration V2 = ml
1000 ml of 1 N thio (1 equivalent) reacts with 127 g (1 equivalent) of Iodine
Therefore, V2 – V1 ml of N normal thio reacts with 127 g of iodine
= g of thio (let it be I)
Iodine value, ie.the number of g
of iodine required by 100 g of the oil =

CHEM LAB-II
PROCEDURE:
DETERMINATION OF ACID VALUE:
Exactly 1g of the oil sample is taken into a 250ml conical flask and 10 ml of
neutral alcohol is added. The content is heated over a water bath for about 30 minutes
and cooled to room temperature. The oil is titrated with the standardized KOH solution
using phenolphthalein indicator until a faint permanent pink colour appears at the end
point. The volume of KOH consumed (V) is taken as the amount of KOH consumed to
neutralize the free acid in the oil sample.
DETERMINATION OF SAPONIFICATION NUMBER:
Exactly 1g of the oil sample is taken into a 250ml conical flask and exactly 20 ml
of standardized KOH is pipetted out into it. The content is heated for about 30 minutes
and cooled to room temperature. This is titrated with the standardized acid solution using
phenolphthalein indicator till a faint permanent pink colour disappears at the end point.
The volume of KOH consumed is noted as V1. Simultaneously, a blank titration under
identical conditions without oil is also performed. The volume of acid consumed in this
blank titration is noted as V2 and the volume difference (V2 – V1) is taken as the amount of
alkali consumed to saponify the oil.
DETERMINATION OF IODINE VALUE:
Exactly 1 g of the oil sample is taken into a 250ml stoppered iodine flask and 20ml
of standardized iodine (in CCl4) is pipetted out into it. The contents are kept in a dark
place with occasional shaking for one hour. The solution is titrated against standardized
sodium thiosulphate till the brown red colour of iodine turns into straw yellow. At this
stage, a few drops of freshly prepared starch indicator solution is added. The titration is
continued till the disappearance of intense blue colour and the volume of thio consumed
is noted as V1.
Simultaneously, a blank is also kept for one hour and titrated against thio using
the same procedure and noted as V2. The volume difference (V2 – V1) is taken as the
amount of iodine consumed by the given oil sample.

CHEM LAB-II

CHEM LAB-II
Result:
A. The different types of alkalinity and TDS present in the given sample is found to
be as follows:
S.No. Type of alkalinity Amount in ppm
1. Phenolphalein
2. Methyl Orange
3. Total alkalinity
4. Hydroxyl ions
5. Carbonate ions
6. Bicarbonate ions
Amount of Total Dissolved Solids (TDS) =
B. Acid value, Saponification number and iodine value of the given oil sample is
found to be as follows :
S.No. Percent
1. Acid Value
2. Saponification Number
3. Iodine Value

CHEM LAB-II

Expt.
Electroplating of nickel & copper and
No.
determination of cathode efficiency
Date
AIM:
Determination of cathode efficiency of nickel and copper electroplating.
Theory:
Electroplating is a widely used metal finishing process to coat a single metal or an

alloy on a conducting substrate. The object to be plated is made as cathode by
connecting it to the negative terminal of the power supply. The plating takes place due to
the reduction of metal ions from the bath solution
Mn+ + ne-→ M
The other electrode, which is connected to the positive terminal becomes the anode
and undergoes dissolution
M →Mn+
The soluble anode replenishes the ions into the bath solution.
The deposition process obeys Faraday’s law. The quantity of metal deposited at the
cathode and the quantity that is dissolved from the anode are directly proportional to the
coulombs of electricity passed. In electroplating works, the following components are
essential
1. An electroplating bath containing the relevant metal ion, electrolytes, complexing

agents and organic additives.
2. Electrically conducting cathode (the article or job)
3. Electrically conducting anode
4. An inert vessel
5. d.c power source
15
CHEM LAB-II
(i) Bath components
Electrolytes are essential for the conductivity of the bath and the buffers are needed
to control the pH at the desired range. Some complexing agents are also added to keep
the deposition at more negative potentials. For example, according to the emf series, the
iron is more active than the copper and hence when iron is in contact with a copper
solution, there would be a spontaneous plating of copper on the iron articles. Such
coatings are very poor, non uniform and would readily peel away. To overcome this
trouble, the complexing agents such as cyanides, hydroxides, and sulphamates are
added which would polarize the deposition potential and ensure that the plating takes
place only during the electrolysis. To obtain desired structural morphological coatings, a
wide range of organic compounds are added as additives in low concentrations.
(ii) Mechanisms of plating:
The deposition mechanism has two distinct stages. At the start of the processes, the
deposition of the metal occurs on the electrode surface and initiates nucleation. Once the
electrode is fully covered by a few atomic layer of the deposited metal, the layer thickens
with macroscopic deposits.The quality of an electrodeposited finish is dependent upon a
wide range of process variables such as electrolyte compositions, additives, pH,
temperature, current density, electrode-cell geometry and flow conditions.
(iii) Applications of electroplating:
Electroplating imparts desired mechanical and physical properties on the article for
specific applications. Some of them are given below.
Metal
Characters Application areas
coating
Cr Hard, wear and corrosion resistant, low friction Steel rolling, hydraulic rams
Food processing machinary,

Ni Soft, solderable, machinable and wear resistant
hydraulic parts
Threaded parts of high temperature

Ag Electrical conductivity, resistant to fretting
machinary
Coatings for internal combustion

Sn Soft and ductile, resistant to abrasive wear
engines
Heavy current bus bars and

Au High electrical conductivity, low contact resistance.
switchgears
Cu Low cost, high electrical conductivity Printed circuit boards
16
CHEM LAB-II
Decorative chrome is almost always plated over either nickel or a copper and
nickel-plated layer. These sub-layers of copper and nickel tend to seal off the substrate
so that the micro-cracking chrome deposit does not present corrosion problems.
1. Surface pretreatment and plating:

In any electrochemical process, the surface pretreatment of the object is very
important. For electroplating, the following operations are carried out during surface
pretreatment.
Mechanical cleaning by wire

Rinsing in Washing
brushing or sand blasting or emery
water pickling
sheet cleaning to remove surface
Drying and weighing. Degreasing in

organic solvents.
After the surface preparation, the cleaned metal is electroplated by keeping it as

the cathode in between two suitable anodes.
2. Current Efficiency of Electroplating Process:
The total amount of chemical change at an electrode is exactly proportional to the
quantity of electricity passing. In the usual electroplating situation, the chemical change of
interest is the quantity of metal deposited at the cathode or dissolved at the anode. Any
other side reactions like hydrogen evolved at the cathode by the reaction
2H2O + 2e → H2 + 2OH-or
oxygen at the anode by the reaction
2H2O → O2 + 4H+(aq) + 4e
represents a waste of electricity and a reduction in the efficiency of the process.
Thus the percentage current efficiency is defined as
Current efficiency (CE) = 100 x Actual weight of metal deposited/Theoritical weight
thetheoritical weight is the weight to be expected from Faraday's laws if there were
no side reactions.
i.e., m =zIt ; where, z = Electrochemical equivalent of Nickel/Copper, I = Current in
Ampere and t = time in seconds.
Cathode efficiency is current efficiency as applied to the cathode reaction, and
anodeefficiency is current efficiency as applied to the anode reaction.
3. Nickel and copper plating:

The nickel plating process is used extensively for decorative, engineering and
electroformingpurposes because the appearance and other properties of
17
CHEM LAB-II
CHEM LAB-II
electrodeposited nickel can be varied over wide ranges by controlling the composition
and the operating parameters of the plating solution.
In the laboratory, nickel is plated on a metal strip using Watt’s bath of the following
composition
Nickel sulphate – 240 g/lit
Nickel Chloride – 60 g/lit
Boric acid – 30 g/lit
where NiSO4 is the main electrolyte, NiCl2 aids in anodic dissolution by preventing its
passivation and boric acid maintains the pH at 5. It is most popular nickel electroplating
solution because of its low cost and simplicity.
During the nickel plating process, the discharge of nickel ions is not the only
reaction that can occur at the cathode; a small percentage of the current is consumed in
the discharge of hydrogen ions from water. This reduces the cathode efficiency for nickel
deposition from 100 per cent to 92 to 97 per cent depending on the nature of the
electrolyte. The discharged hydrogen atoms form bubbles of hydrogen gas at the cathode
surface.
Copper is an excellent choice for an undercoat, since itoften covers minor
imperfections in the base metal. It isrelatively inert in most plating solutions of other
commonmetals; it has a very high plating efficiency, resulting inexcellent coverage even
on difficult-to-plate parts; and lastly,it is highly conductive, making it an excellent coating
forprinted wiring boards or as a coating on steel wire used toconduct electricity.
The plating baths of commercial importancefor electrodeposition of copper are the
alkalinecyanide and pyrophosphate complex ion baths and theacid sulfate and fluoborate
simple ion systems. The most widely used arethe acidic copper sulfate solutions.Deposits
produced in cyanide solutions are typicallythin and are used as an undercoating fornickel
and chromium. Copper deposits from cyanide solutions are not generallysuitable for
deposition of relatively thick deposits for electroformingand similar applications.
In the laboratory, copper is deposited on a metal strip using acid copper bath
having the following composition.
Copper sulphate - 200g/L
Sulphuric acid - 100g/L
where CuSO4 is the main electrolyte and sulphuric acid improves plate characteristics,
increases solutionconductivity, and greatly reduces anode and cathode polarizations. The
acid also prevents the precipitation ofbasic salts.
17
CHEM LAB-II
PROCEDURE:
A strip of metal plate is cleaned with emery sheet, washed with running water, dried
in an oven and then weighed(W1). A convenient area is marked on the plate, and the
current to be supplied for the given current density rating is calculated. The prepared strip
is kept as the cathode in the plating bath such that the marked area is immersed in the
bath solution and two well cleaned metal sheets(metal to be electrodeposited) are used
as anodes and placed on both the sides of the cathode. Definite amperage of current is
passed through the cell for 15 min. The plate is then removed, washed, dried and
weighed (W 2). From the weight of nickel/copper deposited (W 2-W 1), the cathodic
efficiency of nickel/copper plating is calculated. The experiment is simultaneously carried
out for two more samples at different current densities.
Nickel plating
Anode - Nickel
Cathode - the given metal strip
Electrolyte - Waat’s Bath having the following composition
Nickel sulphate – 240 g/lit
Nickel Chloride – 60 g/lit
Boric acid – 30 g/lit
Copper plating
Anode - Copper
Cathode - the given metal strip
Electrolyte - Acid copper bath having the following composition
Copper sulphate - 200g/L
Sulphuric acid - 100g/L
18
CHEM LAB-II
Calculation of Cathode efficiency of Nickel Plating:
Plate I:
2
Current Density = A/dm
Area =
dm 2
Current to be passed for the calculated area = current density in A/dm 2 x Area in dm 2
Weight of metal plate before nickel deposition =
Weight of metal plate after nickel deposition =
Weight of nickel deposited =
Theoretical weight of nickel deposited as per
Faraday’s first law = = ZIt
= 0.3041x 10-3 x current x 900.
Cathode efficiency of nickel plating = Actual weight deposited

100
Theoretical weight
19
CHEM LAB-II
Note:
Electrochemical equivalent of Nickel = Equivalent weight of Nickel/ 965000C
Equivalent weight = Atomic weight / valence = 58.71 / 2 = 29.35
-3
Electrochemical equivalent, Z = 29.35/96500 = 0.3041x 10 g / coulomb
Electrochemical equivalent of copper = Equivalent weight of copper / 965000C
Equivalent weight = Atomic weight/ valence = 63.54/2 = 31.77
-4
Electrochemical equivalent, Z = 31.77 / 96500 = 3.2901x 10 g / coulomb
20
CHEM LAB-II
Plate II:
2
Area =
2
dm
Weight of metal plate before nickel deposition =
Weight of metal plate after nickel deposition =
Weight of nickel deposited =
Theoretical weight of nickel deposited as per
= 0.3041x 10-3 x current x 900.
Cathode efficiency of nickel plating = x 100
21
CHEM LAB-II
Calculation of Cathode efficiency of Copper Plating:
Plate I:
2
Area =
dm 2
Weight of metal plate before Copper deposition =
Weight of metal plate after Copper deposition =
Weight of Copper deposited =
Theoretical weight of Copper deposited as per
= 3.2901x 10-4 x current x 900.
Cathode efficiency of Copper plating = x 100
22
CHEM LAB-II
CHEM LAB-II
Plate II:
2
Area =
dm 2
Weight of metal plate before Copper deposition =
Weight of metal plate after Copper deposition =
Weight of Copper deposited =
Theoretical weight of Copper deposited as per
= 3.2901x 10-4 x current x 900.
Cathode efficiency of Copper plating = x 100
23
CHEM LAB-II
RESULT:
1 The cathode efficiency of nickel plating at a

current density of
2 The cathode efficiency of Copper plating at a

current density of
REVIEW QUESTIONS:
1. State Faraday’s first law of electrolysis.
2. Calculate the amount of copper deposited after passing 0.5 A of current for 8
minutes.
3. Calculate the amount of silver deposited when one coulomb of electricity is passed
through silver nitrate solution?
4. What is the role of a complexing agent in an electroplating bath?
5. What is the advantage of using soluble anodes? What is the need for inert anode in
certain electroplating processes?
6. Nickel chloride is added in small amounts in the watt’s bath though the nickel
sulphate, is the major nickel ion provider. Why?
7. What are the applications of copper and Nickel plating?
8. Why is current efficiency of electroplating process less than 100%?
9. What are the treatment given to the plating effluents before being discharged?
10. What are the pretreatments given to a substrate before electrplating?
24
CHEM LAB-II
CHEM LAB-II
Expt. A Determination of Redwood / Saybolt

No. numbers and kinematic viscosity of
lubricating oils.
Date B Proximate analysis of coal –
determination volatile matter, of
moisture, ash and fixed carbon.
A. Redwood / Saybolt numbers and kinematic viscosity of

lubricating oil
AIM:
To determine the Redwood / Saybolt numbers of the given oil at various temperatures
and to calculate the kinematic viscosity of the oil at the required temperatures.
THEORY
Viscosity is the property of a fluid that determines its resistance to flow. It is an

indicator of flow ability of lubricating oil. Lower the viscosity greater is the flow ability of
the oil. Viscosity is mainly due to the forces of cohesion between the molecules of
lubricating oil. Some liquids have low viscosity and they flow readily, e.g., water, petrol,
kerosene, ether, alcohol, etc. on the other hand, there are some liquids which flow slowly
and have high viscosity, e.g. glycerine, honey, castor oil, liquid polymers, etc.
Viscosity can’t be measured directly. It is usually measured in comparison with a

reference liquid like water. This is called relative viscosity; it is expressed in terms of
coefficient of viscosity. There are two related measures of fluid viscosity - known
as dynamic (or absolute) and kinematic viscosity.
Dynamic (absolute) viscosity (ŋ)
It may be defined as “the tangential force per unit area which is required to
maintain a unit velocity gradient between two parallel layers”. It is denoted by ŋ. Its unit in
CGS system is poise and in SI system is kg/m s.
Kinematic Viscosity
It is the ratio of absolute viscosity to density for any fluid. It is denoted by ν. Its unit
in CGS system is stokes.
ν=µ/ρ
where
ν = kinematic viscosity, µ = absolute or dynamic viscosity and ρ = density.
In the SI-system the unit of kinematic viscosity is m2/s.
25
CHEM LAB-II
FACTORES AFFECTING THE VISCOSITY OF A LIQUID
1.Temperature:
Viscosity of lubricating oil is inversely proportional to temperature. i.e., with

increse of temperature ,viscosity decreases. This is due to the decreases in
intermolecular attraction. At higher temperatures, oils must have sufficient viscosity to
carry loads. Hence , heavier oils are used at higher temperatures. Similarly , light oils are
used at low ambient temperatures.
The rate at which the viscosity of an oil changes with temperature is measured by
an empirical number, known as viscosity index (VI). The low viscosity index shows
relatively large change in viscosity with temperature.
2.Pressure:
At high pressure on the surface of a liquid, the friction between layers increases,
and so viscosity increases. However, for lubricating oil, if the pressure increases at the
surface of a solid, viscosity increases at the interface of the two moving surfaces.
DETERMINATION OF VISCOSITY OF OIL
PRINCIPLE:
The absolute viscosity of fluid oil can be determined by measuring the rate of flow
of the oil through a capillary tube kept at a particular temperature. The specific viscosity of
the given lubricating oil is generally determined by measuring the time taken for a given
quantity of oil to flow through an orifice or jet of standard dimension under standard
conditions.
REDWOOD VISCOMETERS:
1. Redwood viscometer No.1: It is used to measure the viscosities of liquids having

relatively low viscosities, like petrol, kerosene, alcohol, etc. Its jet (capillary)
portion has an inner diameter of 1.62mm and length of 10mm.
2. Redwood viscometer No.2: It is used to measure the viscosities of liquids having

relatively high viscosities, like glycerine, castor oil, etc. It has a jet with an inner
diameter of about 3.8mm and length of 50mm.
DESCRIPTION OF THE APPARATUS:
Redwood viscometer consists of a standard oil cup surrounded by water bath with
electrical heating device. The oil cup is surrounded by a loosely fitting sleeve, which has a
broad flange at the top and fans for stirring the bath. A standard capillary is provided at
the bottom of the tube and the flow through the capillary is controlled by means of a ball-
ended stopper.
26
CHEM LAB-II
1. Oil cup: Cylindrical oil cup made of brass or copper with silver plating on the
inside and open at the upper end. It has a central hole at its bottom having diameter
of about 1.62mm and length 10mm. this can be opened or closed by raising
/dropping a solid brass ball valve fitted with a wire as shown in the figure. Inside the
oil cup, there is a mark up to which oil should be filled in the cup. A thermometer is
dipped into the oil cup fitted with the lid, to note the temperature.
2. Kohlrausch flask: A specially shaped flask with a mark on its neck up to which
the volume is 50cc.It is used to receive the oil after it passes through the orifice of the
oil cup.
SAYBOLT VISCOMETER:
The Saybolt universal-viscometer consists of vertical oil cup of 3 cmdia and 9cm deep
with an orifice 0.1765 cm in diameter in the center of the bottom. The oil cup is supported
in jacket, which serves as container for the oil bath, and is equipped with a stirring device
and an electrical heater. An opening is provided below the discharge orifice into which a
cork is fitted to enable the operator to start the oil flow at any desired instant.
27
CHEM LAB-II
TABULATION
A = 0.0022 & B = 1.88
Temperature ⁰C Redwood / Saybolt Kinematic viscosity

S.No. viscosity number (t)
Initial Final Average seconds k = At – B/t (stokes)
2
8
CHEM LAB-II
DETERMINATION OF REDWOOD / SAYBOLT NUMBER
PROCEDURE:
The oil cup is cleaned well with petrol and filled with the given oil up to the
required level. A sensitive thermometer is inserted into the oil cup through the provision in
the apparatus. The flow time required for the collection of 50cc of the oil through the
standard orifice is noted with the aid of stop clock at room temperature. The water bath is
then slowly heated to raise the temperature of the given test oil and the temperature is
noted. By controlling the temperature (in such a way that the initial and final temperature
readings do not differ more than 5oC), the time required for 50cc outflow of the oil is
noted. The time in seconds is the Redwood/ Saybolt viscosity number of the oil at that
temperature. Similarly Redwood viscosity numbers of the oil for every 10oC rise is noted
o
up to 90 C.
A graph is drawn by plotting viscosity number against the average temperature.

From this graph, the viscosity at the required temperatures is obtained. The kinematic
viscosity is calculated using the following equation,
k = At – B/t
Where, A = 0.0022 and B = 1.8 and t = viscosity number in seconds. A graph between
kinematic viscosity and temperature is also drawn to obtain the kinematic viscosity at the
specified temperature.
PRECAUTIONS:
1. The oil should be filtered before use to remove solid particles that may clog the
capillary of the oil cup.
2. The Kohlrausch flask should be placed just below the jet so that there is no loss of
oil. It is in such a way that the oil stream from the jet strikes the neck of the receiving
flask and does not cause foaming.
3. After each reading the oil should be completely drained out of the receiving flask.
29
CHEM LAB-II
B. Proximate analysis of coal – determination volatile

matter,moisture, ash and fixed carbon.
AIM:
To determine the moisture, volatile matter, fixed carbon and ash contents in a
given coal sample.
THEORY:
Coal is a highly carbonaceous matter that has been formed as a result of

alteration of vegetable matter (e.g., plants) under certain favourable conditions under the
earth. It is chiefly composed of C, H, N and O, besides non-combustible inorganic matter.
The process of conversion of degraded matter into various form of coal is called
coalification. Coal is classified or ranked on the basis of its carbon content.
Anthracite > Bituminous > Sub-bituminous > Lignite > Peat.
This depends on the extent to which the coalification has occurred, the maturity it
has attained in coalification, or age of the coal. The coals on heating, in the absence of
air, become soft, plastic and fuse together to large coherent masses called caking coals.
Consequently, such coals are difficult to be oxidized. If the residue obtained after heating
is porous, hard, and strong and usable for metallurgical purpose, the original coal is
known as coking coal, and the residue is called coke.
STRUCTURE OF COAL:
The structure of coal consists of clusters of aromatic carbon rings with appreciable
amounts of hydroaromatic carbon. An average of 65 to 75 percent of the carbon is
aromatic, 15 to 25 percent is hydroaromatic, and 5 to 10 percent is aliphatic. The
individual clusters are joined together chemically in layers or lamellae by various types of
bonds including short aliphatic bridges (e.g., methylene), ether linkages, sulfide or
disulfide linkages,etc., The lamellae appear to be held together in more or less parallel
layers by physical interactions (e.g., hydrogen bonding or vander Waals forces) in a
"graphite-like" structure.
30
CHEM LAB-II
MOISTURE CONTENT:
Coal is found to be associated with moisture owing to its nature and origin. When
a wet coal is exposed to atmosphere, the external moisture gets evaporated but some
moisture is left with the coal. This moisture is referred as air dried moisture.
Significance
1. Excess moisture in coal is undesirable as it lowers the calorific value of coal by

taking away appreciable amount of the liberated heat in the form of latent heat of
vaporization.
2. Moisture also increases the transport cost.
3. Presence of excessive moisture quenches fire in the furnace.
4. Lesser the moisture content better is the quality of coal as a fuel. However
presence of about 5-10% moisture is desirable as it helps the coal to exist as lumps
and prevents loss of coal which otherwise will escape in the blaze.
VOLATILE MATTER:
The volatile matter in coal consists of a complex mixture of gaseous and liquid
products resulting from the thermal decomposition of the coal. Volatile matter does
not include moisture of coal. It consists of combustible gases such as H₂, CO, CH₄
and other hydrocarbons.
Significance
1. A high percent of volatile matter issued during burning gives a long flame and
produces lot of smoke, some gases may escape unburnt reducing the calorific value.
2. Coals containing less than 20% of volatile matter are not suitable for the
manufacturing of metallurgical coke. Coal with 20-30% of volatile matter will form hard
and strong coke. Coals with >30% volatile matter are used in the manufacturing of
coal gas and tar products.
31
CHEM LAB-II
CALCULATION
MOISTURE CONTENT:
Weight of empty crucible (W 1) = g
Weight of crucible + coal sample before heating (W 2) = g
Weight of crucible + coal sample after heating (W 3) = g
Weight of coal sample (W 2-W 1) = g
Weight of moisture (W 2-W 3) = g
Weight loss due to moisture
Moisture content of the given coal sample (%) = ---------------------------------------- x 100
Weight of coal taken
(W 2-W 3)
= --------------- x 100
(W 2-W 1)
32
CHEM LAB-II
CHEM LAB-II
ASH CONTENT:
Inorganic mineral substances present in coals are converted into ash during
combustion. Ash content is usually a mixture of silica, alumina, iron oxide, magnesia
and residual quantities of lime.
Significance
1. The high percentage of ash is undesirable.
2. The ash does not contribute to the calorific value of coal. But, it reduces the
calorific value and creates many difficulties in efficient utilization of coal.
3. In furnace grid, the ash may restrict the passage of air and lower the rate of
combustion.
4. High content of ash leads to loss of heat energy and cause problems like
clinkering (forming of ash lumps).
FIXED CARBON:
Fixed carbon content increases from low ranking coals such as lignite to high
ranking coals such as anthracite. Higher the percentage of fixed carbon greater is its
calorific value and better is the quality of coal. This represents the quantity of carbon
that can be burnt by a primary current of air.
Significance
1. Higher the percentage of fixed carbon, greater is the calorific value.
2. The percentage of fixed carbon helps in designing the furnace and shape of the
fire-box because it is the fixed carbon that burns in the solid state.
PROCEDURE:
DETERMINATION OF MOISTURE:
In a previously weighed silica crucible (W 1), about 1 gram of coal sample is taken
and weighed accurately (W 2). The crucible along with the coal sample is placed in a hot
air oven at 110°C for 1 hour to remove moisture. It is taken out and cooled in a desiccator
to attain room temperature and weighed again (W 3). From the weight difference, the
percentage of moisture is calculated.
Weight loss due to moisture removal
% of moisture = ------------------------------------------------- x 100
33
CHEM LAB-II
DETERMINATION OF VOLATILE MATTER:
The residual coal in the crucible is covered with a lid and then heated in a muffle
furnace at 900°C ± 25°C for about 20 minutes. The crucible is then cooled on a ceramic
title for few minutes followed by cooling in a desiccator to attain room temperature and
then weighed (W 4). From the weight difference, the percentage of volatile matter is
calculated.
Loss in weight due to removal of volatile matter
% of volatile matter = --------------------------------------------------------------- x 100
Weight of coal sample taken
VOLATILE CONTENT:
Weight of crucible + coal sample after removal of moisture (W 3) = g
Weight of crucible + coal sample after heating (W 4) = g
Weight of coal sample (W 2 – W 1) = g
Weight of volatile matter (W 3 – W 4) = g
Loss in weight due to removal of volatile matte
Volatile matter content (%) = --------------------------------------------------------------- x 100
(W 3 – W 4)
= ------------------- x 100
(W 2 – W 1)
34
CHEM LAB-II
DETERMINATION OF ASH CONTENT:
In a previously weighed silica crucible (W E), about 1 gram of coal sample is taken
and weighed accurately (W S). The crucible along with the coal sample is heated in a
muffle furnace at 725 ± 25°C for nearly half an hour. The crucible is then cooled on a
ceramic title for few minutes followed by cooling in a desiccator to attain room
temperature and then weighed (W A). From the weight difference, the percentage of ash is
calculated.
Weight of ash left
% of ash content = ---------------------------- x 100
PRECAUTIONS:
1. After air drying the coal the weighing should be done quickly so as to prevent
absorption of atmospheric moisture by the sample.
2. If black particles of unburnt carbon appear in the crucible even after heating for 30
minutes in the electric Bunsen ,heating should be continued for another 15 minutes.
35
CHEM LAB-II
ASH CONTENT:
Weight of empty crucible (W E) = g
Weight of crucible + coal sample (W S) = g
Weight of crucible + coal sample after burning (W A) = g
Weight of coal sample (W S-W E) = g
Weight of ash left (W A-W E) = g
Weight of ash left
Ash content of the given coal sample (%) = ---------------------------- x 100
(W A-W E)
= ---------------------- x 100
(W S-W E)
FIXED CARBON:
Fixed carbon (%) = 100 - [% of Moisture content +Volatile matter + Ash content]
37
CHEM LAB-II
Result:
A. Variation of viscosity of the given lubricating oil with temperature is

studied.
The Kinematic viscosity

of the given oil at
B. Proximate Analysis of the given Coal sample contains the following:
S.No. Percent
1. Moisture Content
2. Ash Content
3. Volatile Content
4. Fixed Carbon Content
REVIEW QUESTIONS:
1. Why is proximate analysis so called?
2. Calculate the mass and volume required for the combustion of 1Kg of carbon.
3. What is fixed carbon? How is it measured?
4. Write the combustion equation of carbon.
5. What is the average ash content of an Indian coal?
6. What is fly ash? Write its drawbacks.
7. What is coke?
8. Differentiate between caking coals and coking coals.
9. Define calorific value.
10. Differentiate between HCV & LCV.
38
CHEM LAB-II
CHEM LAB-II
Expt. A Determination of efficiency of corrosion

No. inhibitor.
Date B Determination of flash, fire cloud and
pour points of an oil sample.
A.Determination of efficiency of corrosion inhibitor.
AIM:
To determine the inhibitor efficiency of hexamine on the corrosion rate of mild steel
in acid media by weight loss method.
THEORY : CORROSION
PRINCIPLE:
Corrosion is defined as the deterioration or destruction of materials by chemical or

electrochemical interaction with their environment. The well known examples are rusting
of iron – reddish brown scale formation on iron and steel objects. It is very slow and
inward process and starts from the surface of a metal. The corrosion phenomenon is a
just “reverse process of extraction of metals”.
1. Chemistry of Corrosion
Why do metals undergo corrosion: Most of the metals (except noble metals
like Au, Pt etc) exist in nature in their combined forms like oxides, carbonates, sulphates
etc. In combined form they have lower energy. The pure or isolated metals have high
energy so they are thermodynamically unstable. Due to this reason metals have
tendency to acquire the thermodynamic stability i.e. lower energy. For this, metals easily
undergo interaction with their environment either chemically or electrochemically to from a
stable compound by the process of corrosion. Due to corrosion metal has lost its
malleability, ductility and electrical conductivity etc. Hence we can simply say that
corrosion is just “reverse extraction of metals”.
Corrosion
Metal Metallic Compound
+Energy
(High Energy) (Lower Energy)
Metal Extraction
Virtually all corrosion reactions are electrochemical in nature. At the anodic surface
iron goes into solution as ferrous ions. As iron atoms undergo oxidation to ions, they
release electrons and the negative charge builds up in the metal and prevents further
39
CHEM LAB-II
anodic reaction, or corrosion. Thus this dissolution will only continue if the electrons
released in a cathodic reaction. At the cathodic site, the electrons are taken up by
species of the electrolyte.
The most common and important electrochemical reactions in the corrosion of iron
are thus
Anodic reaction:
1. Fe → Fe2+ + 2e─
Cathodic reaction:
+ ─
2. 2H + 2e → H2(g) ( at acidic pH)
─ ─
3. H2O +½O2 + 2e → 2OH ( at neutral and alkaline condition)
2+ ─
4. Fe + 2OH → Fe(OH)2↓
If enough O2 is present iron (II) hydroxide is further oxidized to form rust.
5. 2Fe(OH)2 + H2O + ½O2 → 2 Fe(OH)3
6. 4 Fe (OH)3 → 2Fe2O3. H2O + 4H2O ( Dehydration)
Rust
Corrosion of the material is otherwise called as million dollar thief. So prevention of

corrosion is of vital concern.
7. Corrosion Prevention
Corrosion can be prevented or reduced by retarding either the anodic or cathodic

reactions. This can be achieved in several ways:
1. Conditioning the Metal: Covering of base metal with other metal or paints and
mixing of one metal with other metal or nonmetal i.e. alloy forming.
2. Electrochemical Control: Sacrificial anodic and current impressed methods.
3. Conditioning the Corrosive Environment:
1. Removal of oxygen from the corrosive environment: This can be

achieved by adding suitable reducing agent e.g. Na2SO3.However, for open
evaporative cooling systems this approach to corrosion prevention is not
suitable since fresh oxygen from the atmosphere will have continual access.
40
CHEM LAB-II
CHEM LAB-II
2. By using corrosion inhibitors: A corrosion inhibitor is a chemical additive,

which, when added to a corrosive aqueous environment, reduces the rate of
corrosion. It can function in one of the following ways:
1. Anodic inhibitors – as the name implies an anodic inhibitor interferes

with the anodic process. Inhibitor reacts with metal ions and it forms
insoluble compounds. These precipitate forms a protective film and
prevents corrosion. If an anodic inhibitor is not present at a
concentration level sufficient to block off all the anodic sites, localized
attack such as pitting corrosion can become a serious problem.
Example: Chromates, nitrite,etc.
2. Cathodic inhibitors: the major cathodic reaction is the reduction of

oxygen or evolution of hydrogen gas. Corrosion rate can be controlled
by antimony and arsenic oxides. Slowing down of the diffusion of the H +
ions, can be achieved by adding amines, pyridines.
3. Adsorption type corrosion inhibitors– many organic inhibitors

work by an adsorption mechanism. The resultant film of chemisorbed
inhibitor is responsible for protection either by physically blocking the
surface from the corrosion environment or by retarding the
electrochemical processes. The main functional groups capable of
forming chemisorbed bonds with metal surfaces are amino (-NH2),
carboxyl (-COOH), and phosphonate (-PO3H2).
In practical conditions it is not usually possible to eliminate completely all corrosion

damage to metals used for the construction of industrial plant. The rate at which attack is
prime importance is usually expressed in one of two ways:
1. Weight loss per unit area per unit time, usually mdd (milligrams per square
decimetre per day)
2. A rate of penetration, i.e. the thickness of metal lost. This may be expressed in mpy
(milli inches penetration per year) or mm/y.
For example in the case of corrosion of heat exchanger tubes in industrial cooling
water a typical corrosion rate in untreated water would be 40-50 mpy; the use of a
corrosion inhibitor could reduce this to less than 5 mpy. The mild steel tubing used in
heat exchangers is a maximum of 200 thousandths of an inch thick, thus with corrosion
rates of 40-50 mpy in untreated water, severe problems might be expected within four or
five years. If suitable water treatment with corrosion inhibitors is used a life of at least
twenty years might be expected. When designing equipment for a certain service life,
engineers often add a “corrosion allowance” to the metal thickness, permitting a certain
amount of thinning before serious weakening occurs. In a cooling water system the
factors influencing the rate of attack are:
41
CHEM LAB-II
S.No. Factors influencing corrosion rate Causes
The condition of the metal surface Corrosion under the deposits, with a possibility of pitting (severe attack in
1
corrosion debris and other deposits small spots)
The nature of the environment

In the range of 4-10 corrosion rate is fairly independent of pH, but it
increases rapidly when the pH falls below 4.
2 1. pH
2. Availability of oxygen Increase in oxygen concentration usually gives an increase in corrosion rate.
Increased water flow increases oxygen access to the surface and removes
3 Flow rate protective surface films, so usually increases corrosion, but can sometimes
improve access for corrosion inhibiting reactants.
Very important, in general low corrosion rates are found with scale-forming
(hard) waters. Aggressive ions which accelerate corrosion are Cl─, SO 2-
4 Water type 4
but quite complex interactions may occur between the various dissolved
species in natural waters.
Determination of Corrosion rate:
A specimen is exposed to the corrosive medium for a specified time and the weight
of the specimen noted before and after exposure. The corrosion rate is calculated from
the weight loss using the formula.
Corrosion rate = mpy
Where, W - Weight loss of the specimen in mg,

3
D - Density of mild steel (7.8 g/cm )
A - Area of the mild steel in sq. inch,
T - Exposure time in hour.
By exposing a specimen with and without the inhibitor in a corrosive media, the
efficiency of the inhibitor can be measured.
Let A be the corrosion rate without inhibitor and B as the corrosion rate in the
presence of corrosion inhibitor.
Then, the inhibitor efficiency = X 100
42
CHEM LAB-II
Determination of Corrosion rate:
A specimen is exposed to the corrosive medium for a specified time and the weight
of the specimen noted before and after exposure. The corrosion rate is calculated from
the weight loss using the formula.
Corrosion rate = mpy
Where,
W - Weight loss of the specimen in mg,

3
D - Density of mild steel (7.8 g/cm )
A - Area of the mild steel in sq. inch,
T - Exposure time in hour.
By exposing a specimen with and without the inhibitor in a corrosive media, the
efficiency of the inhibitor can be measured.
Let A be the corrosion rate without inhibitor and B as the corrosion rate in the
presence of corrosion inhibitor.
Then, the inhibitor efficiency = X 100
43
CHEM LAB-II
DETERMINATION OF CORROSION RATE AND INHIBITOR EFFICIENCY
Area of the Initial Final

Concentration of Weight Corrosion Inhibitor
plate weight of weight of
S.No the inhibitor loss rate efficiency
the plate the plate
(Sq.
(ppm) (mg) (mpy) (%)
inches) (g) (g)
1. Blank-I ---
2. Blank-II
3.
4.
5.
6.
7.
Calculation:
Area of the plate = l x b x 2 sq.inches.
Corrosion rate = mpy (milli-inches penetration per year)
The inhibitor efficiency = X 100
44
CHEM LAB-II
CHEM LAB-II
PROCEDURE:
The experiment involves the following steps.
Exposure to Measurement of
Specimen environment change in
preparation (with and without specimen weight.
inhibitor)
The given mild steel plates are cleaned according to the following steps.
1. Pickling with 40% hydrochloric acid (by volume) to remove the oxides if any, washing
with running water and drying with filter paper.
2. Polishing the plates with emery sheets followed by washing with running water.
3. Degreasing with acetone.
4. Drying with hair drier or in hot air oven at 120o C.
The pretreated plates are weighed accurately (W 1) and the dimensions are measured.
One of the plates is completely immersed in the given corrosive media that does not contain
inhibitor. Other plates are immersed in the media of the same strength but with different
inhibitor (hexamine) concentrations for the specified time (the inhibitor concentrations can be
100 ppm, 200 ppm, 300ppm etc.). Then the specimens are removed, washed well with
running water, dried and weighed (W 2). The corrosion rate is calculated from the weight loss
of the specimens with and without inhibitors. From the corrosion rate measurements, the
inhibitor efficiency is calculated using the above formula.
45
CHEM LAB-II
REVIEW QUESTIONS:
1. In a small town along the coastal area, it is observed that iron objects rust easily.
Identify the factor which contributes to this rusting phenomenon.
2. Iron pieces are dipped in 1M HCl and 1M H2SO4 solutions separately. Which one
corrodes faster? Why?
3. Write a short-hand description of the reactions involved in the corrosion of zinc in acid
medium.
4. What is the chemistry involved in corrosion of iron in acid medium?
5. Describe a simple method to reduce the corrosion due to dissolved oxygen in a water
container or vessel.
6. When platinum and silver are electrically connected in an electrolytic bath, which one
gets corroded?
7. What are the factors that affect the corrosion process?
8. What is cathodic protection?
9. What is galvanic corrosion?
10. Write the formula to calculate the corrosion rate.
11. What is the unit of corrosion rate?
12. W hat are the different inhibitors used to reduce corrosion rate?
13. W hat is meant by electrochemical corrosion?
46
CHEM LAB-II
B. Determination of flash, fire cloud and pour points of an

oil sample.
AIM:
To determine the flash and fire point, cloud and pour point temperatures of the
given sample of lubricating oil.
THEORY:
The flash point of the lubricating oil is defined as the lowest temperature at which it
forms vapours and produces combustible mixture with air. The higher flash point
temperature is always desirable for any lubricating oil. If the oil has the lower value of flash
point temperature, it will burn easily and forms the carbon deposits on the moving parts. The
difference between flash and fire point temperatures may vary from 20°C to 60°C. The flash
and fire point temperatures depends upon the volatility of the oil. The flash point of some
fuels are given below
Fuel Flash Point (0C) Auto ignition

Temperature (0C)
Ethanol (70%) 16.6 363
Gasoline (petrol) -43 280
Diesel >62 210
Jet fuel >60 210
Kerosene (paraffin oil) >38-72 220
Vegetable oil (canola) 327
Biodiesel >130
DESCRIPTION OF THE APPARATUS: FLASH AND FIRE POINT
The Cleveland open cup apparatus consists of a cylindrical cup of standard size. It
is held in position in the metallic holder which is placed on a wire gauge. It is heated by
means of an electric heater housed inside the metallic holder. A provision is made on the top
of the cup to hold the thermometer. A standard filling mark is done on the inner side of the
cup and the sample of oil is filled up to the mark.
47
CHEM LAB-II
DESCRIPTION OF APPARATUS : CLOUD AND POUR POINT
The cloud and pour point of lubricating oil is determined with the help of ‘cloud and
pour point apparatus. It consists of the following parts:
Flat bottomed cylindrical vessel having 3cm in diameter and 12cm height is
surrounded by a air jacket which is placed in a cooling chamber containing freezing mixture.
The freezing mixture has the composition of either ice & salt or ice and CaCl2 or solid CO2
and petrol based on the requirement of cooling temperature. A thermometer is inserted in
the cooling bath to measure the temperature.
48
CHEM LAB-II
CLOUD POINT:
It is the temperature at which the oil becomes cloudy or hazy in appearance when it
is cooled in a standard apparatus at a standard rate. Lubricating oils which are derived from
petroleum contain dissolved paraffin wax and other asphaltic or resinous impurities. The
amounts of these impurities may vary depending upon the source and refining process
employed. At low temperatures i.e. when oil is cooled down, these impurities tend to
separate out of the oil in the form of minute crystals that result in cloudiness.
POUR POINT:
It is the temperature at which the oil just ceases to flow when cooled at a standard
rate in a standard apparatus. If, after the cloud point, the oil is cooled further, more and more
of impurities will crystallize and a stage is reached where the oil becomes a gel. Thus pour
point can also be defined as the lowest temperature at which oil starts to flow or pour under
such a cooled and undisturbed conditions. Pour point depressing additives are phenol and
certain condensation products of chlorinated wax with naphthalene. These prevent the
separation of wax from the oil.
Significance:
The cloud point and pour point indicate the suitability of a lubricant in cold conditions.
1. The lubricating oils used in capillary feed systems or wicking arrangement should
have low cloud points, otherwise at low temperatures the crystals of impurities will
separate out clogging the capillary or wick interstices.
2. In the fuel intake system of diesel engine, the lubricants having high cloud points may
clog the filter screens.
3. A high pour point leads to the solidification of the lubricant that may cause jamming
of the machine.
4. Pour point also gives an idea of the lowest temperature at which oil can be
transferred by pouring.
5. Pour point determines the suitability of oil for low temperature installations which may
be required to start and operate at sub-zero temperatures. Examples refrigerator plants
and air craft engines.
6. For refrigeration systems, oil with low pour point, low viscosity and low cloud point is
needed .So naphthenic base oils, possessing such characteristics are mostly used. The
0 0
pour point requirements are -40 F (maximum) for the lightest grade and -13 F for the
heaviest grade oils. Their viscosity range is 85 to 325 SUS (Saybold Universal
Seconds) at1000F.
49
CHEM LAB-II
PROCEDURE FOR THE DETERMINATION FLASH AND FIRE POINT:
The cup is cleaned with petrol and filled with oil up to the mark. The cup is
placed in position and thermometer is kept inside the oil such that the bulb of the
thermometer is ¼” from the bottom of the cup. The oil is heated at a rate of 5⁰C per minute.
The test flame is applied for every 3⁰C rise in temperature. W hen a flash appears any point
on the surface of oil, the temperature is noted as the flash point. The heating is continued at
the same rate until the test flame ignited the oil and it continues to burn at least for 5
seconds. This temperature is the fire point of the oil.
PRECAUTIONS:
1. The oil cup must be cleaned and dried properly so that it is free from moisture, as
moisture affects the flash point.
2. The bulb of the thermometer should be inside the oil.
3. Oil should be filled up to the mark.
PROCEDURE FOR THE DETERMINATION OF CLOUD AND POUR POINT:
The given oil is filled up to the mark inside the flat bottomed glass tube and the cork is
then fitted. The bulb of the thermometer should be dipped beneath the oil level. The tube is
then kept in the freezing mixture to decrease the temperature of the oil. The tube is taken out
of the freezing mixture after every 1⁰C fall in temperature and then inspected for a moment.
It is restored if the cloudiness has not formed. The temperature is recorded as cloud point at
which on inspection cloudiness in the oil is witnessed. The cooling is further continued. After
every 1⁰C fall of temperature, the tube is then withdrawn and tilted to see the flow of the oil
for 30 seconds. If there is some movement of the oil, the test tube is replaced immediately in
the jacket. The temperature at which, no movement of the oil takes place is recorded as the
pour point of the oil.
PRECAUTION:
The complete operation of the removal and replacement of the test jar should be completed
within 3 seconds.
50
CHEM LAB-II
REVIEW QUESTIONS:
1. Define flash point and fire point.
2. Give any two differences between flash point and fire point.
3. W hy is measuring the flash point of oil necessary?
4. W hy should the oil in Cleveland open cup apparatus be free from moisture?
5. If the oil has the lower flash point, what does it indicate?
6. If the oil contains moisture, how can it be dried?
7. Define cloud and pour point of a liquid lubricant.
8. How can the pour point of oil be lowered?
9. W hat are the significance of pour point and cloud point determination?
10. W hat are pour points depressant?
11. “Lubricating oil used in refrigerators should have lower cloud and pour points “- justify.
12. W hat is meant by a freezing mixture?
---------------------
51
CHEM LAB-II
RESULT:
A. The given inhibitor efficiency on the corrosion rate at different concentration is

determined as follows:
Concentration of
Plate No. inhibitor in N HCl Inhibitor efficiency (%)
(ppm)
B. The flash, fire, cloud and pour points of the given oil is found to be
Flash point
1
Fire point
2
Cloud point
3
Pour point
4
52

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CHEMISTRY LABORATORY MANUAL

(Common to Production / Mechanical – G1 Branches)

Course code 15P212 / 15M212

Course title CHEMISTRY LAB – II

BRANCH PRODUCTION / MECH-G1 ENGINEERING

PSG COLLEGE OF TECHNOLOGY

Dr. SENTHILKUMAAR/CHEM PROD/MECH-G1

PSG COLLEGE OF TECHNOLOGY

BRANCH PRODUCTION / MECH-G1 ENGINEERING

CERTIFIED BONAFIDE RECORD OF WORK DONE BY

Date Signature of the faculty

Dr. SENTHILKUMAAR/CHEM PROD/MECH-G1

Dr. SENTHILKUMAAR/CHEM PROD/MECH-G1

S.No Name of the Experiments Page

A Determination of alkalinity and TDS of water.

Electroplating of Nickel & Copper, and determination of cathodic

Determination of Redwood / Saybolt numbers and kinematic viscosity

A Determination of efficiency of corrosion inhibitor.

Dr. SENTHILKUMAAR/CHEM PROD/MECH-G1

GENERAL RULES OF LABORATORY SAFETY

1. Avoid keeping mobile phones during the laboratory hours.

4. Do not perform any unauthorized experiments.

5. Students at this level must not work alone in this laboratory.

8. Always notify the instructor in case of an injury.

Dr. SENTHILKUMAAR/CHEM PROD/MECH-G1

Marks obtained Sign.

Dr. SENTHILKUMAAR/CHEM PROD/MECH-G1

3. Read the principle and experimental procedure of assigned experiment before

5. Experiment number and date should be entered at the beginning of every

6. All entries must be made directly with a non-erasable ink/ball pen.

9. Plan the organization of the data in your laboratory manual.

10. Write all observations/readings only in the laboratory manual.

Dr. SENTHILKUMAAR/CHEM PROD/MECH-G1

Marks obtained Sign.

Dr. SENTHILKUMAAR/CHEM PROD/MECH-G1

Dr. SENTHILKUMAAR/CHEM PROD/MECH-G1

Expt. A Determination of alkalinity and TDS of water.

A. Determination of alkalinity and TDS of water.

The alkalinity of a water sample is a measure of its capacity to neutralize acids.

Dr. SENTHILKUMAAR/CHEM 2 PROD/MECH-G1

Alkalinity causing ions

2. [P]= [M] [P] or [M] 0 0

3. [P]= ½ [M] 0 2[P] or [M] 0

4. [P] > ½ [M] 2[P] - [M] 2[M] - 2[P] 0

5. [P] < ½ [M] 0 2[P] [M] - 2[P]

Dr. SENTHILKUMAAR/CHEM 3 PROD/MECH-G1

Standard sodium carbonate Vs hydrochloric acid

Burette solution : Hydrochloric acid

Volume of sodium Burette readings (ml)

Volume of sodium carbonate solution V1 = ml

Normality of sodium carbonate solution N1 = N

Volume of hydrochloric acid solution V2 = ml

Normality of hydrochloric acid solution N2 = V 1 N1 / V 2

Dr. SENTHILKUMAAR/CHEM 4 PROD/MECH-G1

TITRATION I: STANDARDIZATION OF HYDROCHLORIC ACID

Exactly 20 ml of standard sodium carbonate solution is pipetted out into a clean

TITRATION II: ESTIMATION OF ALKALINITY

Equivalent weight of CaCO3 is 50 g

Equivalent weight of Na2CO3 is 53.g

Dr. SENTHILKUMAAR/CHEM 5 PROD/MECH-G1

Titration II: Estimation of alkalinity in water

Concordant value (i). P = ml

Dr. SENTHILKUMAAR/CHEM 6 PROD/MECH-G1

DETERMINATION OF TOTAL DISSOLVED SOLIDS (TDS):