LABORATORY MANUAL

4330504
CHEMICAL PROCESS TECHNOLOGY

Semester – III

Diploma in Chemical Engineering

Government Polytechnic
Gandhinagar
 GOVERNMENT POLYTECHNIC GANDHINAGAR
CHEMICAL ENGINEERING DEPARTMENT

CERTIFICATE

This is to certify that

Mr./Ms __________________________________________________

Enrollment No. ________________ Branch Diploma in Chemical

Engineering Semester: _______ has satisfactorily completed the course

in the subject CHEMICAL PROCESS TECHNOLOGY (4330504) in

the year ___________

Date of Submission: ____________

In Charge Faculty Head of Department

Institute Vision:
To Develop Technically Proficient & Ethically Sound Diploma Engineers Contributing to
Industry & Society Needs.

Institute Mission:
Government Polytechnic, Gandhinagar Strives,
1. To impart quality technical education.
2. To shape students towards sensitizing in ethical values and contributing in nature.
3. To familiarize students with the world of work.

Vision of Department:
To Prepare Competent Diploma Chemical Engineers.

Mission of Department:
 To provide the fundamental knowledge of chemical engineering and operation ability through
outcome based chemical engineering education.
 To provide opportunities to student to find out inherent interpersonal skills and high moral
values through extracurricular and co-curricular activities.
 To provide opportunities to students for institute industry interaction through different
initiatives.

Program Education Objectives (PEOs):

Diploma chemical engineer will be able to

 Apply operational skills, laboratory skills, analytical skills and critical thinking by the use of
fundamental knowledge of science & engineering.
 Demonstrate the high level of interpersonal skills and high moral values in working
environment.
 Demonstrate responsibility towards environmental, safety and social aspect.

Program Outcome (POs):

PO1: Basic and Discipline specific knowledge: Apply knowledge of basic mathematics, science and
engineering fundamentals and engineering specialization to solve the engineering problems.
PO2: Problem analysis: Identify and analyze well-defined engineering problems using codified
standard methods.
PO3: Design/ development of solutions: Design solutions for well-defined technical problems and
assist with the design of systems components or processes to meet specified needs.
PO4: Engineering Tools, Experimentation and Testing: Apply modern engineering tools and
appropriate technique to conduct standard tests and measurements.
PO5: Engineering practices for society, sustainability and environment: Apply appropriate
technology in context of society, sustainability, environment and ethical practices.
PO6: Project Management: Use engineering management principles individually, as a team member
or a leader to manage projects and effectively communicate about well-defined engineering activities.
PO7: Life-long learning: Ability to analyze individual needs and engage in updating in the context of
technological changes.
Program Specific Outcome (PSOs):

PSO1: An ability to operate Chemical Process considering economic, environmental, health safety and
sustainability aspects.
PSO2: Be able to conduct lab experiment, analyze and communicate the results effectively.

Course Outcomes (COs):

Course Statement
Outcome After successful completion of the course, student will be able to
C204.1 Explain the classification and properties of various chemicals.
Apply concept of the manufacturing processes of various chemicals with neat
C204.2
sketch to operate chemical plant.
C204.3 Identify major engineering problems encountered in manufacturing processes.
C204.4 Suggest applications of various chemicals.

Course
PO1 PO2 PO3 PO4 PO5 PO6 PO7 PSO1 PSO2
Outcome
C204.1 3 - - 2 - 2 1 - -
C204.2 3 2 - 3 2 2 2 2 3
C204.3 2 2 - - 2 - - 2 -
C204.4 2 - - 1 1 - 1 - -

Average 2.5 2 - 2 1.7 2 1.3 2 3

 INDEX

Sr. Relevant Page Sign of Marks

List of Experiments Date Remarks
No. CO No. Faculty (10)

1 Standardize Sulfuric Acid Solution C204.1 1

C204.2,
2 Preparation of Hydrated Lime C204.3, 5
C204.4

C204.2,
3 Preparation of Caustic Soda C204.3, 11
C204.4

C204.2,
4 Preparation of Potassium Chloride C204.3, 17
C204.4

C204.2,
5 Preparation of Phenol Formaldehyde C204.3, 23
C204.4

6 Find out Acid Value of Oil C204.1 27

C204.2,
7 Preparation of Soap C204.3, 31
C204.4

C204.2,
8 Preparation of Detergent Powder C204.3, 35
C204.4

Find out moisture, volatile matter C204.1

9 39
and ash content in fuel

10 Determine Calorific Value of Fuel C204.1 45

C204.2,
11 Preparation of Aspirin C204.3, 51
C204.4

C204.2,
12 Prepare of Nitrobenzene C204.3, 55
C204.4
 EXPERIMENT - 1
STANDARDIZATION OF SULFURIC ACID SOLUTION

AIM: To prepare 0.1 N H2SO4 solution & standardize it using 0.1 N NaOH solution.

APPARATUS:

 Beaker
 Burette with stand
 Conical Flask
 Measuring Cylinder
 Pipette
 Glass Rod
 Weight Box

CHEMICALS:

 H2SO4
 NaOH
 Distilled Water
 Phenolphthalein Indicator

PROCEDURE:

1. Prepare 0.1 N H2SO4 & 0.1 N NaOH solution.

2. Fill the burette with 0.1 N NaOH solution.
3. Take 10 ml of H2SO4 solution in a conical flask.
4. Add 2-3 drops of Phenolphthalein indicator in it.
5. Titrate it with 0.1 N NaOH solution.
6. Note down the readings when end point (colorless to pink color) is reached.
7. Find out normality of the solution.

1
OBSERVATION:

1. N1= Normality of NaOH solution = ______ N.

2. V1= Volume of NaOH solution = ______ ml.

3. V2= Volume of H2SO4 solution = ______ ml.

OBSERVATION TABLE:

Sr.
Burette reading Differences Average
No.
(Final – Initial) (ml) (ml)
Initial (ml) Final (ml)

CALCULATIONS:

N1V1 = N2V2

Where,

N1= Normality of NaOH solution

N2= Normality of H2SO4 solution

V1= Volume of NaOH solution

V2= Volume of H2SO4 solution

N2 = N1V1
V2

2
RESULT: Normality of Prepared H2SO4 Solution is _______N.

CONCLUSION:

QUIZ:
1. What is the purpose of titration?

2. What is normality?

3. Calculate equivalent weight of H2SO4 & NaOH.

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity

2 Discipline

3 Performance

4 Documentation

5 Safety

Total (10)

3
4
 EXPERIMENT - 2
PREPARATION OF HYDRATED LIME

AIM: To Prepare Hydrated Lime from Quick Lime.

APPARATUS:

 Pre-mixing chamber or vessel

 Air separator
 Screw conveyor
 Dryer

CHEMICALS:

 Quicklime
 Distilled Water

THEORY:

The lime is consisting essentially either of CaO to gather with a smaller proportion of MgO,
formed by burning a natural rock (like lime stone, CaCO3) at such a temperature that it will slake,
when brought in contact with water.

Lime is a high melting white solid when water is added to pure lime (called quick lime) lumps; it
is readily absorbed through the pores forming Ca (OH) 2

CaO + H 2O → Ca (OH) 2 + 15.9 kcal

This change is called slaking or hydration. The slaking of lime is accompanied:

(i) evolution of a considerable amount of heat ( about 2.25 kcal/kg)

(ii) expansion in volume to 2-2.5times
(iii) development of “hissing & cracking sound”
Due to (a) Conversion of water into stream
(b) Breaking of lime to extremely fine white powder, called slaked lime.
Thus slaked lime is extremely fine white powder, obtained by the absorption of water by lime.
For making Mortar/plaster, lime in “slaked lime” form is used

The lime is most commonly supplied by mgf. In hydrated lime form (i.e. a fine white powder,
obtained by adding limited amount of water to lime) because it
(i) It is easier to handle
(ii) It can be stored with less danger
(iii) It can be used immediately
(iv) It comes with greater safety because of much less evolution of heat
(v) It is pure calcium limes are poorly plastic, rather sticky and hard to work
5
OBSERVATION:
1. Theoretical amount of hydrated lime= ___________gm.
2. Practical amount of hydrated lime= ___________gm.

CALCULATION :

Theoretical Yield Hydrated Lime:

Molecular Weight of CaO = 56 g/mol

Molecular Weight of Ca(OH)2= 74 g/mol

So,

1 mole of CaO gives 1 Mole of Ca(OH)2

56 g CaO gives 74 g of Ca(OH)2

2 g CaO gives 2.64 g of Ca(OH)2

Theoretical Yield = 2.64 g

Practical Yield = ___________g

Percentage yield of Hydrated Lime = Practical Yield X 100

Theoretical Yield

6
PROCEDURE:

1. Proceed by the slow addition of water to crushed or ground 2 gm quick lime in a premixing
chamber or a vessel known as a hydrator, both of which mix and agitate the lime and water.
2. The amount of water added is critical. Too much water makes it impossible, or too costly,
to produce the desired dry form.
3. Too little water leaves incomplete, causing degraded quality, namely chemical instability
and structural unsoundness.
4. More than this theoretical amount (24.5%) of moisture is necessary to counteract the loss
of moisture as stream generated by the appreciable heat of hydration.
5. In practice, about 50-65% water is added, depending on the degree of reactivity of the quick
lime and its physical size.
6. The finest particles hydrate most rapidly after hydration, the slightly moist slaked lime is
propelled by an enclosed screw conveyer to an air separator, where the coarse fraction is
largely removed as tailings.
7. This step enhances the fineness of the powder, up grading its chemical purity and dries the
powder further.
8. The hydrate may be further refined or conveyed to a silo for bagging in 22.7 kg paper stalks
or for bulk truck or rail-car shipment.

RESULT: Yield of Hydrated Lime produced =_______%

CONCLUSION:

QUIZ:
1. What is Yield?

2. What are the uses of lime?

7
8
3. What is molecular formula of hydrated lime?

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity

2 Discipline

3 Performance

4 Documentation

5 Safety

Total (10)

9
10
 EXPERIMENT - 3
PREPARATION OF CAUSTIC SODA

AIM: To prepare the caustic soda by chemical method.

APPARATUS:

 Weighing balance
 Measuring cylinder
 Burette with stand
 Pipette
 Beaker
 Glass Rod

CHEMICALS:

 Soda ash (Sodium carbonate)

 Calcium hydroxide
 Hydrochloric acid
 Distilled water
 Phenolphthalein indicator

THEORY:

Sodium hydroxide, also known as lye and caustic soda, is an inorganic compound with the
formula NaOH.
It is a white solid ionic compound consisting of sodium cations Na + and hydroxide anions OH−.
Sodium hydroxide is a highly caustic base and alkali that decomposes proteins at ordinary
ambient temperatures and may cause severe chemical burns. It is highly soluble in water, and
readily absorbs moisture and carbon dioxide from the air.
It forms a series of hydrates NaOH·nH2O. The monohydrate NaOH·H2O crystallizes from water
solutions between 12.3 and 61.8 °C. The commercially available "sodium hydroxide" is often this
monohydrate, and published data may refer to it instead of the anhydrous compound.
As one of the simplest hydroxides, sodium hydroxide is frequently used alongside
neutral water and acidic hydrochloric acid to demonstrate the pH scale to chemistry students.
Sodium hydroxide is used in many industries: in the manufacture
of pulp and paper, textiles, drinking water, soaps and detergents, and as a drain cleaner.
Worldwide production in 2004 was approximately 60 million tons, while demand was 51 million
tons.
11
OBSERVATIONS:

1. Normality of Hydrochloric acid solution. N1 = _____N

2. Volume of sample of clear solution taken for titration (V1) = ____ml
3. Final burette reading (V2) = ______ ml
4. Total volume of clear solution (V) = _____ ml

CALCULATIONS:

Theoretical Yield Calculation:

Na2CO3 + Ca (OH) 2 2 NaOH + CaCO3

For each gmol

grams 106 74 2*( 40) 100

So, by Stoichiometric equation,

1 mole (=106 gms) of Sodium Carbonate produces 2 mole (=80 gms) of Sodium Hydroxide

Therefore, 10.6 gms of Sodium carbonate will produce

y = (10.6*80)/106 gm

= ______ gm

Practical Yield Calculation:

Normality of sodium hydroxide solution:

N2 
N1 V1
N2 
_____  _____ 
V2 _____

N2  N

Now,

gm equivalent
Normality 
lit of solution

gm equivalent = Normality x lit of solution

= ______x_____

= ______gm eq.
12
Sodium hydroxide is a popular strong base used in industry. Sodium hydroxide is used in the
manufacture of sodium salts and detergents, pH regulation, and organic synthesis. In bulk, it is
most often handled as an aqueous solution, since solutions are cheaper and easier to handle.
Sodium hydroxide is used in many scenarios where it is desirable to increase the alkalinity of a
mixture, or to neutralize acids.
For example, in the petroleum industry, sodium hydroxide is used as an additive in drilling mud to
increase alkalinity in bentonite mud systems, to increase the mud viscosity, and to neutralize
any acid gas (such as hydrogen sulfide and carbon dioxide) which may be encountered in
the geological formation as drilling progresses.
Another use is in Salt spray testing where pH needs to be regulated. Sodium hydroxide is used
with hydrochloric acid to balance pH. The resultant salt, NaCl, is the corrosive agent used in the
standard neutral pH salt spray test.

PROCEDURE:

1. Take 10.6 gm of Soda ash accurately by weight scale.

2. Weight 7.4 gm of Calcium hydroxide and add it with soda ash in a beaker with 200 ml of
distilled water.
3. Mix the content of the beaker.
4. Put the beaker on the heating mental and heat it for about 30 minutes. During heating stir the
content continuously.
5. After heating allow the solution to settle down the precipitates.
6. Separate the clear solution careful from the precipitates.
7. Take 10ml of clear solution in a conical flask and titrate it against 0.1 N HCl solution.
8. Use phenolphthalein as indicator. At the end color change is from pink to colorless.
9. Measure the volume of clear solution.

RESULT: The percentage yield of Sodium Hydroxide = _______ %

CONCLUSION:

13
Weight of Solute = gm equivalent x Eq. weight of solute

Practical Yield(x) = ______ gm

Percentage Yield of Sodium Hydroxide obtained = x 100

14
QUIZ:

1. What are the different methods used in industry to produce caustic soda?

2. List down the five major industries of Gujarat producing caustic soda.

3. List out various application of caustic soda.

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity

2 Discipline

3 Performance

4 Documentation

5 Safety

Total (10)

15
16
 EXPERIMENT - 4
PREPARATION OF POTASSIUM CHLORIDE

AIM: To Prepare Potassium Chloride.

APPARATUS:

 Beaker
 Measuring Cylinder
 Conical Flask
 Glass Rod
 Weight Box
 Burette with stand
 Filter Paper
 Evaporating Dish

CHEMICALS:

 Potassium Hydroxide
 Phenolphthalein Indicator
 HCl
 Distilled Water

THEORY:

Potassium chloride (KCl, or potassium salt) is a metal halide salt composed

of potassium and chlorine.

It is odorless and has a white or colorless vitreous crystal appearance. The solid dissolves
readily in water, and its solutions have a salt-like taste. Potassium chloride can be obtained
from ancient dried lake deposits.

KCl is used as a fertilizer, in medicine, in scientific applications, domestic water softeners (as
a substitute for sodium chloride salt), and in food processing, where it may be known as E
number additive E508.

It occurs naturally as the mineral sylvite, and in combination with sodium

chloride as sylvanite. Potassium chloride is extracted from minerals sylvite, carnallite,
and potash.

It is also extracted from salt water and can be manufactured by crystallization from
solution, flotation or electrostatic separation from suitable minerals.
17
OBSERVATION:

1. Weight of Potassium Hydroxide taken = W1 = _______gm.

2. Weight of Potassium Chloride (Practical Yield) = W2 = ______gm.

CALCULATION:

Theoretical Yield of Potassium Chloride:

KOH + HCl = KCl + H 2O

56 gm 36.5 gm 74.6 gm

56 gm. of Potassium Hydroxide is yielding 74.6 gm. of Potassium Chloride

.
While W1 gm. of Potassium Hydroxide is yielding =

=
Theoretical Yield = _______gm.

Percentage Yield of Potassium Chloride = x 100

18
 It is a by-product of the production of nitric acid from potassium nitrate and hydrochloric acid.

The vast majority of potassium chloride is produced as agricultural and industrial grade potash
in Saskatchewan, Canada, as well as Russia and Belarus.

Saskatchewan alone accounted for over 25% of the world's potash production in 2017.

Potassium chloride is inexpensively available and is rarely prepared intentionally in the

laboratory. It can be generated by treating potassium hydroxide (or other potassium bases)
with hydrochloric acid:

KOH + HCl → KCl + H2O

This conversion is an acid-base neutralization reaction. The resulting salt can then be purified
by recrystallization. Another method would be to allow potassium to burn in the presence of
chlorine gas, also a very exothermic reaction.

PROCEDURE:

1. Take 50 ml of 2.0 M Potassium Hydroxide in conical flask.

2. Add 2-3 drops of Phenolphthalein indicator in it.
3. Fill the burette with 2.0 M HCl solution.
4. Now, add HCl into the conical flask slowly while swirling it.
5. Continue adding until the color of the solution in the flask changes from pink to colorless.
6. Pour the content of the conical flask into evaporating dish. Heat the mixture to evaporate
water.
7. Now let the mixture cool at room temperature.
8. Filter the mixture to obtain potassium chloride crystal.
9. Wash the crystal using distilled water.
10. Dry the crystal & measure it weight.

RESULT: Percentage yield of potassium chloride obtained is ______%.

CONCLUSION:

19
20
QUIZ:

1. What is fertilizer?

2. Write down the uses of potassium chloride.

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity

2 Discipline

3 Performance

4 Documentation

5 Safety

Total (10)

21
22
 EXPERIMENT - 5
PREPARATION OF PHENOL FORMALDEHYDE

AIM: To Prepare Phenol Formaldehyde.

APPARATUS:

 Beaker
 Measuring Cylinder
 Conical Flask
 Glass Rod
 Weight Box
 Water Bath

CHEMICALS:

 Phenol
 40% Formaldehyde solution
 Distilled Water
 HCl
 Glacial acetic acid

CHEMICAL REACTION:

THEORY:

1. Phenol formaldehyde is formed by condensation polymerization.

2. It is prepared by condensing phenol with formaldehyde solution in the presence of acid or
alkaline catalyst.

Applications:
Main uses fall into three class
1. Resin + solvent = it is used in coating , varnishes
2. Resin + water = it is used in adhesive bonding
3. Solid resin = it is used in all types of thermo set molded solid form.

23
24
PROCEDURE:
1. Place 5 ml of glacial acetic acid and 2.5 ml formaldehyde solution in a beaker.
2. Add 2 gm phenol and 1 ml of conc. HCl in it.
3. Heat slowly and constantly for 5 minutes.
4. A large mass of pink plastic is formed.
5. The residue is washed several times with distilled water.
6. Filter the product and dry it in oven.
7. Weigh the dry product and calculate yield of phenol formaldehyde.

RESULT: The weight of obtained phenol formaldehyde is _______ g.

CONCLUSION :

QUIZ :
1. What is Polymer?

2. What are the uses of phenol formaldehyde?

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity
2 Discipline
3 Performance
4 Documentation
5 Safety
Total (10)

25
26
 EXPERIMENT-6
FIND OUT ACID VALUE OF OIL

AIM : To Determine the Acid Value of Given Oil Sample.

APPARATUS:
 Weighing balance
 Heater
 Conical flask
 Burette with stand
 Measuring Cylinder

CHEMICALS:
 Oil Sample
 Sodium hydroxide
 Neutral Alcohol (Absolute Alcohol)
 Phenolphthalein indicator

THEORY :
 Acid value indicates the proportion of free fatty acid present in an oil or fat.
 Acid value defined as the number of milligrams of caustic potash required to neutralize the
acid in 1 gm of the sample.
 The normal acid value for most samples lies within 0.5. If any acid other than a fatty acid
is present in the sample, it will be an error. A high acid value indicates a stale oil or fat
stored under improper conditions.
 The acid number is a measure of the number of carboxylic acid groups (−C(=O)OH) in a
chemical compound, such as a fatty acid, or in a mixture of compounds.
 In a typical procedure, a known amount of sample dissolved in an organic
solvent (often isopropanol) and titrated with a solution of alcoholic potassium hydroxide
(KOH) of known concentration using phenolphthalein as a colour indicator.

PROCEDURE :
1. Weigh 5 gm of oil and transfer it into 250 ml conical flask.
2. Add 50 ml of neutralized alcohol in it.
3. Heat this mixture for 15 minutes.
4. Take the solution after 15 minutes and add 1 or 2 drops of phenolphthalein indicator.
5. Titrate this against the NaOH solution from the burette.
6. The appearance of pink color indicates the end point.
27
OBSERVATION:

1. Weight of Oil sample = ______gm.

2. Final volume of titration = _____ml.
3. Normality of NaOH = _____N.

CALCULATION:

Acid value = 5.61 x Volume of NaOH

Weight of Oil sample

Acid Value =

28
RESULT: The acid value of the given oil sample was found to be______.

QUIZ:
1. What is Acid Value?

2. Write the importance of Acid Value?

3. Why Phenolphthalein is used?

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity

2 Discipline

3 Performance

4 Documentation

5 Safety

Total (10)

29
30
 EXPERIMENT - 7

PREPARATION OF SOAP

AIM: To Prepare Soft Soap Bar from Coconut Oil.

APPARATUS:

 Measuring cylinder
 Beaker
 Glass rod
 Weight box
 Evaporating disc

CHEMICALS:

 Coconut oil
 Water
 NaOH
 Perfumes
 Color

THEORY:

 Soap comprises of the sodium or potassium salts of various fatty acids like oleic, stearic
acid, palmitic, lauric & stearic acid, tallow, coconut oil, palm oil, grease is raw material for
soap.
 The soap from coconut oil is firm & lathers well. It contains large properties of very
desirable glycerides of lauric & stearic acid.
 The main classes of soap are toilet soap & industrial soaps. Toilet soaps are made from
selected materials & nearly contains 15 to 20% moisture, showing soaps contains a
considerable property of potassium soap and an excess of stearic acid.
 The combination giving a slower drying latter.

PROCEDURE:

1. Take 20 gm coconut oil in beaker.

2. Take 6 gm Sodium hydroxide pellets in to another beaker. Add 10 ml distilled water in it.
3. Add NaOH solution to oil slowly and stir it well, during the addition, saponification
reaction takes place.
4. After compete addition, stir the mix for 20 to 25 min. Add color & perfume.
5. Transfer the mix to evaporating disc and cool the content for 24 hour then weight the
soap bar.
31
OBSERVATION:

1. Weight of oil taken x = ______gm.

2. Weight of sodium hydroxide taken y = ______gm.
3. Volume of water taken z = ______ml.
4. Weight of soap formed a = _______gm.

32
RESULT: The weight of the soap obtained was found to be = ______gm.

CONCLUSION:

QUIZ :
1. Which chemical process used in production of soap?

2. Difference between oil soap and detergent soap?

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity

2 Discipline

3 Performance

4 Documentation

5 Safety

Total (10)

33
34
 EXPERIMENT - 8

PREPARATION OF DETERGENT POWDER

AIM: To Prepare Detergent Powder from Acid Slurry.

APPARATUS:

 Beaker
 Weight box
 Glass rod
CHEMICALS:

 Acid slurry = 20 %
 Sodium Tripoly Phosphate = 30 %
 Sodium sulfate = 25 %
 Sodium carbamate = 10 %
 Borax =6%
 Sodium silicate = 7.5 %
 Sodium carboxyl methyl cellulose = 1.5 %

PROCEDURE:

1. To make 500 g of detergent powder, take 100 g acid slurry and 37.5 g of sodium silicate in
the beaker, then mix it properly.
2. Then take 150 g of sodium tripoly phosphate, 125 gm sodium sulfate, 50 gm of Na 2CO3,
30 gm of borax and 7.5 g of carboxyl methyl cellulose then, add this substance one by one
in that beaker which is already having the mix of acid slurry and sodium silicate on
completion of adding all substance in beaker, mix them.
3. Keep it in dryer for 2 hours. Measure the weight of detergent powder.

RESULT: Weight of detergent powder obtained =_______gm.

CONCLUSION:

35
36
QUIZ:
1. What is chemical name of acid slurry?

2. How detergent works?

3. What are the uses of detergent?

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity

2 Discipline

3 Performance

4 Documentation

5 Safety

Total (10)

37
38
 EXPERIMENT - 09
DETERMINE MOISTURE, VOLATILE MATTER AND ASH CONTENT IN COAL

AIM: To Determine Moisture, Volatile Matter and Ash Content of the Given Coal Sample.

APPARATUS:

 Eclectic Oven
 Muffle Furnace
 Weighing Balance
 Silica Crucible with air tight lid
 Asbestos hand gloves
 Desiccator

CHEMICALS:
 Coal Powder

THEORY:
 Coal is coming in various quality. It is classified mainly on the basis of the fixed carbon and
its heating value.
 Coal is widely used from domestic purpose of heating to its various application in the industries
like in power generation, in mfg. of organic chemicals.
 Coal is analyzed to its quality before coal is taken into use.
 Coal is analyzed in two ways.
1) Proximate analysis
2) Ultimate analysis
 Proximate analysis is the simplest way of analyzing the coal. The following contents are found
in analysis.
1) Fixed Carbon
2) Volatile Matter
3) Moisture
4) Ash (Mineral Matter)
 Ultimate analysis is the specific method of analyzing the coal. The following contents are
found out.
1) Carbon
2) Hydrogen
3) Nitrogen
4) Oxygen
5) Sulphur
6) Its Heating Value

39
OBSERVATION:
1. Weight of the empty crucible = a = _____ gm.
2. Weight of a lid = b = _____ gm.
3. Weight of the crucible with the sample = c = _____gm.
4. Weight of the crucible after heating up to 110 0C. = d = _____gm.
5. Weight of the crucible after heating up to 900 0C. = e = _____gm.
6. Weight of the crucible after heating up to 815 0C. = f = _____gm.

CALCULATION:
1. Weight of crucible with sample and the lid = w = a+b+c = _____gm.
2. Weight of moisture gone out = (w-d) = _____gm.
3. Weight of the volatile matter gone out = (d-e) = _____gm.
4. Weight of the ash remaining after the final heating = f-(a+b) = _____gm.
5. Moisture fraction in the sample = (w-d)/c = x* 100 = ______%
6. Volatile Matter fraction in the sample = (d-e)/c =y* 100 = ______%
7. Ash fraction in the sample = (f-(a+b))/c = z* 100 = ______%

40
PROCEDURE:
1. Measure weight of empty crucible and lid.
2. Take accurately weighed 2 gm of sample coal powder in the crucible and total weight is
noted.
Moisture Content:
3. Place the open crucible with sample in an electric oven and heat it at about 105 –110 0C
for 30 minute to remove the moisture.
4. Now the crucible is taken out carefully and is kept in the deccicator with CaCl 2 to cool
down up to room temp. Then whole crucible is weighed again and weight is noted down.
Volatile Matter:
5. The closed crucible is then heated in a Muffle furnace maintained at 900 0C for 7 minutes
to remove the volatile matter.
6. Crucible is taken out and is kept in the deccicator to cool down up to room temp. Crucible
is again weighed and note down the weight.
Ash content:
7. Place the open crucible with sample in a Muffle furnace maintained at 725 ± 25o C for
about 40 minutes or till constant weight is obtained.
8. Again, Crucible is taken out and is kept in the deccicator to cool down up to room temp.
Crucible is again weighed and note down the weight.

RESULT:

1. Moisture = _____%
2. Volatile Matter = _____%
3. Ash Content = _____%

CONCLUSION:

41
42
QUIZ:
1. List out types of coal.

2. What is the purpose of coal analysis?

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity

2 Discipline

3 Performance

4 Documentation

5 Safety

Total (10)

43
44
 EXPERIMENT NO – 10

DETERMINE CALORIFIC VALUE OF COAL

AIM: To Determine Calorific Value of Fuels By Using Bomb Calorimeter.

APPARATUS:

 Bomb Calorimeter

CHEMICALS:

 Fuel Sample
 Distilled Water

THEORY:

 The “calorific value or heating value” of the fuel is defined as the energy liberated by the
complete oxidation of a unit mass or volume of a fuel. It is expressed in kJ/kg for solid and
liquid fuels and kJ/m3 for gases.
 The higher heating value, HHV, is obtained when the water formed by combustion is
completely condensed.
 The lower heating value, LHV, is obtained when the water formed by combustion exists
completely in the vapour phase.

BOMB CALORIMETER:
 The calorific value of solid and liquid fuels is determined in the laboratory by ‘Bomb
calorimeter’.
 It is so named because its shape resembles that of a bomb. Fig. 1 shows the schematic
sketch of a bomb calorimeter.
 The calorimeter is made of austenitic steel which provides considerable resistance to
corrosion and enables it to withstand high pressure.
 In the calorimeter is a strong cylindrical bomb in which combustion occurs. The bomb has
two valves at the top.
 One supplies oxygen to the bomb and other releases the exhaust gases.
 A crucible in which a weighted quantity of fuel sample is burnt is arranged between the
two electrodes as shown in Fig. 1.
 The calorimeter is fitted with water jacket which surrounds the bomb.
 To reduce the losses due to radiation, calorimeter is further provided with a jacket of water
and air.
 A stirrer for keeping the temperature of water uniform and a thermometer to measure the
temperature up to an accuracy of 0.001°C are fitted through the lid of the calorimeter.

45
CALCULATION:

The heat released by the fuel on combustion is absorbed by the surrounding water and the
calorimeter.
From the above data the calorific value of the fuel can be found in the following Way
Let Wf = Weight of fuel sample (kg),
W = Weight of water (kg),
C = Calorific value (higher) of the fuel (kJ/kg),
We = Water equivalent of calorimeter (kg),
T1 = Initial temperature of water and calorimeter,
T2 = Final temperature of water and calorimeter,
Tc = Radiation corrections, and
c = Specific heat of water.

Heat released by the fuel sample = Wf × C

Heat received by water and calorimeter = (W w + We) × c × [(T2 – T1) + Tc].

Heat lost = Heat gained

Wf × C = (W + We) × c × [(T2 + T1) + Tc]

 Hydrogen will therefore be condensed.

 The procedure of determining calorific values of liquid fuels is similar to that described
above.
 However, if the liquid fuel sample is volatile, it is weighed in a glass bulb and broken in a
tray just before the bomb is closed.
 In this way the loss of volatile constituents of fuels during weighing operation is prevented.

46
 Figure: Bomb calorimeter.

PROCEDURE:

1. To start with, about 1 gm of fuel sample is accurately weighed into the crucible and a fuse
wire (whose weight is known) is stretched between the electrodes.
2. It should be ensured that wire is in close contact with the fuel.
3. To absorb the combustion products of sulphur and nitrogen 2 ml of water is poured in the
bomb.
4. Bomb is then supplied with pure oxygen through the valve to an amount of 25 atmosphere.
5. The bomb is then placed in the weighed quantity of water, in the calorimeter.
6. The stirring is started after making necessary electrical connections, and when the
thermometer indicates a steady temperature fuel is fired and temperature readings are
recorded after 1/2 minute intervals until maximum temperature is attained.
7. The bomb is then removed; the pressure slowly released through the exhaust valve and the
contents of the bomb are carefully weighed for further analysis.

47
48
QUIZ:
1. What do you mean by combustion?

2. What is calorific value?

3. Which coal has highest calorific value?

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity

2 Discipline

3 Performance

4 Documentation

5 Safety

Total (10)

49
50
 EXPERIMENT - 11
PREPARATION OF ASPIRIN

AIM: To Prepare Aspirin from Salicylic Acid.

APPARATUS:
 Weighing Balance
 Conical Flask
 Glass Rod
 Measuring Cylinder
 Filter paper
 Water Bath

CHEMICALS:
 Salicylic Acid
 Acetic Anhydride
 Concentrated Sulphuric Acid
 Distilled Water

THEORY:
By Acetylation of Salicylic Acid using Acetic Anhydride and Concentrated Sulfuric Acid, Aspirin
(Methyl Salicylate) is obtained.

By heating Aspirin it will decompose therefore its specific melting point is found out clearly. It is
decomposed in the range of 1280C to 1350C.

PROCEDURE:
1. 5 gm. of Salicylic Acid is accurately weighed. The weighed quantity of Salicylic Acid is
taken in the conical flask.
2. 7.5 gm. of Acetic Anhydride is accurately weighed and is taken in the same flask. (7.5 gm.
of Acetic Anhydride is equivalent to 7 ml. of Acetic Anhydride.)
3. 3 drops of Concentrated Sulphuric Acid is added in the flask and the flask is shaken well.
4. The flask is heated up to 500C-600C over Water Bath for 15 minutes.
5. The flask is allowed to cool and is shaken at some time interval.
6. 75 ml. of Distilled Water is added in flask and is shaken rigorously.
7. The whole content is filtered.
8. The material is dried and is weighed accurately. The weight of crystallized material is noted
as W1.
51
OBSERVATION:

1. Weight of Salicylic Acid is taken = W3 = ______gm.

2. Weight of Acetic Anhydride is taken = W4 = ______gm.
3. Weight of Aspirin (Practical Yield) = W1 = ______gm.

CALCULATION:

Theoretical Yield of Aspirin:

For 1 gmol
COOH
COOH
OH [ H2SO4 ] OCOCH 3

+ ( CH3CO )2O

119 gm. 102 gm. 178 gm.

119 gm. of Salicylic Acid is yielding 178 gm. of Aspirin

While W3 gm. of Salicylic Acid is yielding = (W3 * 178)/ 119 = ______gm of Aspirin
Theoretical Yield = _______gm.

Percentage Yield of Aspirin obtained = x 100

52
RESULT: Percentage Yield of Aspirin =______%

CONCLUSION:

QUIZ:

1. Write down uses of Aspirin.

2. Write down raw material used for manufacturing of Aspirin.

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity

2 Discipline

3 Performance

4 Documentation

5 Safety

Total (10)

53
54
 EXPERIMENT - 12

PREPARATION OF NITROBENZENE FROM BENZENE

AIM: To Prepare Nitrobenzene from Benzene.

APPARATUS:

 Conical flask
 Water bath
 Measuring cylinder
 Separating funnel
 Thermometer
 Round Bottom flask
 Gravity Bottle
 Beaker

CHEMICALS:

 Nitric Acid (HNO3)

 Sulphuric Acid (H2SO4)
 Benzene
 Distilled Water

THEORY: The nitration reaction serves to introduce one or more nitro groups into a reading
molecule, HNO3, H2SO4 known as mixed acid is most common nitrating medium.

HNO3 + 2 H2SO4 → NO2+ + H3O+ + 2 H2SO4-

The nitrating agent is an electrophillic aromatic substitution reaction hence reaction

will be favored at the carbon atom of aromatic rings, where the electron density is
greatest when the aromatic compound to be nitrated contains a substituent’s the
nitro group can enter at the ortho, meta & para position, contain substitute cause
the electron density to be greater at the ortho or para then at the meta position hence
they held nitration product in which ortho-para isomers.

C6H5H + NO2+ → C6H5HNO2

C6H5HNO2 + HSO4 → C6H5NO2 + H2SO4

The nitration reaction is highly exothermic.

55
OBSERVATIONS:

1. Volume of conc. H2SO4 solution = _______ml.

2. Volume of conc. HNO3 solution = _______ml.
3. Volume of conc. C6H6 solution = _______ml.
4. Specific gravity of C6H6 solution = _______.
5. Specific gravity of H2SO4 solution = _______.
6. Specific gravity of HNO3 solution = _______.
7. Volume of Nitrobenzene obtained = _______ml.
8. Specific gravity of Nitrobenzene = _______.

CALCULATION:

Weight of C6H6 = vol of C6H6 x sp. Gravity

Practical Yield:

Weight of Nitrobenzene obtained = vol. of C6H6 x sp. Gravity

Theoretical yield:

C6H6 + HNO3 + H2SO4 → C6H5NO2 + H2 O + H2SO4

gm C6H6 N.B.
78 → 123
→ ?
=
=

Percentage Yield of Nitrobenzene obtained = x 100

=
56
 Properties:

(1) N.B. is pale yellow liquid

(2) Strong smell of bitter almond
(3) Insoluble in water, soluble in organic solvent
(4) Its vapor is poisonous
(5) M.P. = 5.7 0C, B.P. = -210 0C
(6) Mol. Wt =123 g/ mole

Applications:

Used as solvents, dyestuffs, explosives, pharmaceuticals, and as intermediate for

the preparation of amines. In the mfg. of floor polyester.

PROCEDURE:

1. Take 35 ml of HNO3 in 250 ml Round Bottom flask & add 40 ml of conc. H 2SO4 in it.
2. Keep the mix cooled by immerging it in cold water bath, place a thermometer (0-100 0C)
in a mix.
3. Then add slowly & carefully drop by drop 30 ml of benzene stir the mix occasionally &
maintain the temp. of mix. at 50-55 0C.
4. When the addition is complete, heat the flask in a water bath. Maintain the temp. at 60 0C
for 45 min, stir the mix continuously till the reaction complete.
5. After completion of nitrogen reaction contents of the flask are cooled & transfer into
separating funnel.
6. The lower layer contains acid (spent) which is to be withdrawn in a beaker.
7. The upper Nitrobenzene layer is washed with water & allows settling in a beaker.
8. Collect Nitrobenzene & measure it volume.
9. Measure the gravity of nitrobenzene using gravity bottle.

RESULT:

1. Theoretical Yield = ________gm.

2. Practical Yield = ________gm.

3. Percentage Yield = _______%

57
58
CONCLUSION:

QUIZ :
1. What is specific gravity?

2. What are the properties of nitrobenzene?

3. What are the uses of nitrobenzene?

Assessment Rubrics
Sr.
Criteria Marks
No.
1 Regularity

2 Discipline

3 Performance

4 Documentation

5 Safety

Total (10)

59