CHEMICAL PROCESS

TECHNOLOGY
LABORATORY MANUAL
5th Semester

Department of Chemical Engineering

School of technology
Pandit Deendayal Petroleum University
Gandhinagar
 Chemical Process Technology

CONTENTS:
Sr. Name of the experiment Page. Remarks
no No.
1 To prepare hydrated lime from the given calcium 3-4
carbonate powder.
2 To prepare caustic soda by chemical method. 5-6
3 To prepare soap in the laboratory and to carry out its 7-8
cost analysis.
4 To evaluate the saponification value of given oil 9-10
sample
5 To prepare detergent in the laboratory and to carry out 11-12
its cost analysis.
6 To determine the acid value of given oil samples. 13-14
7 Synthesis of Biodiesel 15-16
8 To prepare Acetanilide from Aniline. 17
9 To prepare m-dinitrobenzene from Nitrobenzene. 18
10 To prepare Benzoic acid from Toluene. 19
11 To prepare Anthraquinone from Anthrancene. 20
12 To prepare sulphanilic acid from aniline. 21
13 To Prepare Salicylic Acid From Methyl Salicylate. 22-23
14 To find the purity of sulfa drug. 24-25
15 To prepare Phenylazo-2-Napthol 26-27
16 To determine the amount of potassium in the given 28
sample of fertilizer.
17 To determine the total insoluble residue in the cement 29
sample.
18 To determine the amount of calcium in the given 30
sample of fertilizer volumetrically.
19 Analysis of Na2CO3 andNaHCO3 mixture 31-32
20 Analysis of bleaching powder 33-34
21 Proximate analysis of Coal 35-37
22 Determination of the Sodium Carbonate in the 38-39
Washing Soda
23 Analysis of cement 40
24 Estimation of silica in cement 41-42

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 2

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Experiment No.: 1

Aim: - To prepare hydrated lime from the given calcium carbonate powder.

Apparatus: - Silica crucible, Muffle furnace, Beaker, Titration set, etc.

Chemicals: - 0.1N HCl, Phenolphthalein, Water. Etc.

Theory: -

Limestone is a constituent of earth, is a rock of sedimentary origin. It’s most

important chemical characteristics is that when subjected to high temperature, it
decomposes into lime which also releases CO2 (decarbonation), the product is known as
quicklime and can be hydrated or slaked in a hydrated lime Ca(OH)2.
CaCO3 → CaO + CO2
(Lime stone) (Quick lime)

CaO + H2O → Ca(OH)2 + Heat

There are three essential factors in the thermal decomposition of limestone.

 The stone must be heated at dissociation temp. of its carbonates.

 The minimum temperature must be maintained for specific duration.
 CO2 evolved must be removed rapidly.

Production is in rotary or vertical kiln, although most lime is sold as quicklime. Production of
hydrated lime is also substantial and is manufactured by the slow addition of water to crushed
lime in a hydrator or agitator, the amount of water added is critical.

Properties: -

Mol Wt.: 74.10 gm/gm mole

Density: 2.2 gm/cc
Decomposition of CaO: 580C
Solubility in water: 0.18 % at 0C, 0.08 % at 100C

Procedure: -

1. Take 2 gm of calcium carbonate powder in a silica crucible, which is weighed previously.

2. Now keep the crucible in a muffle furnace until it comes up to the derived temperature
that is nearly 750C.
3. Now take out the crucible and keep it in glass-desiccator containing Ca(OH)2 in the
bottom so that it attains the room temperature.

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4. Now weigh the crucible with product and find out weight of product.
5. Take out the product in a beaker and add 100 ml of water to it. Prepare solution of lime
forming Ca(OH)2.
6. Test with pH paper if it is found to be basic and note down the pH of the solution.
7. Titrate it against 0.1 N HCl to get gm/lit of Ca(OH)2 present.

Data: -
▪ Calcium carbonate taken = ___________________.
▪ Weight of crucible + substance:
Before heating = _____________.
After heating = _____________.
▪ Weight of CO2 evaporated = ____________________.
▪ Amount of 0.1 N HCl required to titrate Ca(OH)2 = _________________.

Calculations: -

▪ Theoretical yield of first reaction: CaCO3 → CaO + CO2

▪ Theoretical yield of second reaction: CaO + H2O → Ca(OH)2
▪ Weight of mixture after heating:
▪ Normality of Ca(OH)2
▪ gm/lit of Ca(OH)2
▪ Amount of Ca(OH)2
▪ Percentage yield:

Result: -

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 4

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Experiment No.: 2

Aim: - To prepare caustic soda by chemical method.

Apparatus: - Steam bath, Stirrer, Weight box, Beaker.

Chemicals:- Soda ash, Calcium hydroxide, Dilute HCl.

Theory: -

Caustic soda is originally made by the causticization of soda ash with lime.

Na2CO3 + Ca(OH)2 → 2NaOH + CaCO3

The process being no longer employed due to incomplete reaction, loss of efficiency and other
difficulties. Now it is being produced by electrolysis of aqueous solution of alkali metal
chlorides. Pure anhydrous NaOH is a white brittle, crystalline solid. It is highly corrosive to
soluble in water and alkaline.
Molecular weight: 40 g/mol
Melting point: 30C
Boiling point: 139C

The major use of NaOH is to form sodium salt thus neutralizing strong acids and soluble
water insoluble chemicals. It finds use in the soap, textile, petroleum refining and chemical
industries.
Material used for handling and transportation: Nickel is used but it is costly while mild steel is
suitable material.
Solubility of NaOH is 40% at room temperature.

Procedure: -

1. Take 10.6 gm of soda ash in 250 ml beaker and heat it to boiling by means of steam with
7.4 gms calcium hydroxide in 200 ml water.
2. The mixture is kept stirring for about an hour and heated simultaneously.
3. Take a portion of the clear solution and titrate it against dilute HCl.
4. Withdraw the clear solution of NaOH, evaporate it and dry it.
5. Find the gms/lit of NaOH by titrating it against 0.5 N HCl using phenolphthalein as an
indicator.

Observations and Calculations: -

▪ Titration reading =

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▪ Normality of NaOH = NHCl X VHCl

VNaOH

▪ gm/lit of NaOH = NNaOH X Equipment weight.

▪ gm of NaOH obtained = Volume of solution X gm/lit

By reaction,
106 gm of soda ash gives ----------------80 gm of NaOH
10.6 gm of soda ash gives ----------------?
So by stoichiometric proportions, 106 gm of soda ash produces 80 gms of NaOH.

Result: -

The percentage yield of NaOH = _______________.

Conclusion: -

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 6

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Experiment No.: 3

Aim: - To prepare soap in the laboratory and to carry out its cost analysis.

Apparatus: - Beaker, Stirrer, Steam bath, weight box, Measuring cylinder,

Absorbent.

Chemicals: - Oil, NaOH, NaCl.

Theory: -

Soaps are defined as salt of long fatty acids. Most common soaps are of Na and K salts.
Ammonium, amine and heavy metals soaps are also included. Soap is produced using
following reaction.

3NaOH + (C17H35COO)3C3H5 → 3C17H35COONa + C3H5(OH)3

caustic glyceryl sodium glycerin
soda stearate stearate

Most of the marketable soaps are beads of coconut oil of follow.

The surface activity of soap results from soap molecule having a hydrophobic hydrocarbon
group at one end and hydrophilic carboxylic group at the opposite end. These special
properties are used in soil removal.
In the aqueous solution this results in the formalin of oriented hydrophobic change pointing
outward. In the body of the solution the soap molecule aggregate into micelle. This
phenomenon is responsible for dispersing and emulsifying. Properties that make soap solution
are such that they remove soil particles. In the hard water soap forms precipitates of calcium
and magnesium which reduce the activity.

Procedure: -

Take 100 gm of oil in 500 ml beaker. In another beaker prepare 100 ml of 20 % slurry of
NaOH.

Hot Process: -

Heat both the beakers simultaneously on the steam bath of hot plate. When the beakers
attain same temperature add aqueous NaOH to the oil with stirring slowly. Then during the
process when hydrolysis is complete add NaCl to salt out the soap. Separate the soap from
glycerin and leave it dry. The soap is obtained.

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Cold Process: -

With continuous stirring of oil, NaOH solution is added till two layer of solid soap in
glycerin are separated. Add little amount of salt and stir again and allow settling. Then
separate outs the upper layer and dry and weigh it. Then find out its cost/kg.

Result: -

Total amount of soap =

Total cost of soap =

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 8

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Experiment No:4

Aim:- To evaluate the saponification value of given oil sample

Principle:-

The saponification value is the number that expresses in milligrams the quantity of potassium
hydroxide required to neutralise the free acids and to saponify the esters present in 1 g of the
substance.
The term saponification is the name given to the chemical reaction that occurs when a vegetable
oil or animal fat is mixed with a strong alkali. The products of the reaction are two: soap and
glycerine. Water is also present, but it does not enter into the chemical reaction. The alkali used in
modern soap is either potassium hydroxide, which is used to make soft soap or liquid soap
because of its greater solubility, or sodium hydroxide, which is used to make bar soap.

Apparatus Required:-

Erlenmeyer flasks 250ml, Burette, Hot plate, Funnel and filter paper, Analytical balance,
Graduated cylinder 25 ml. Volumetric pipettes (Class A) 20 ml,

Reagents Required:-

Alcoholic potassium hydroxide 0.5 N in ethanol, Hydrochloric acid 0.5N, Phenolphthalein

indicator solution 0.1% in ethanol, DI water, Ethyl alcohol 95%, Methylene blue.

Procedure:-

1. Take 3 ml (2gms.) of given oil sample into an Erlenmeyer flask. Record the weight.
2. Pipette 25 ml of 0.5N Alcoholic KOH into the flask.
3. Heat and reflux the contents for 40 minutes without allowing the vapours to escape out of the
flask
4. After refluxing allow the solution to cool to room temperature.
5. Stir the reaction mixture with the glass rod.
6. Add three to five drops of phenolphthalein indicator to the solution with moderate agitation.
7. Add titrant 0.5N HCL to the burette, and note level.
8. Add titrant from the burette to the solution until the faint pink colour permanently (for at least
thirty seconds) disappears.
Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 9
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9. Note the level of titrant in the burette.

10. Calculate saponification value.

Calculations:-

Sample weight =

Titrant Vol. (TV) = (Titrant volume in step 7) - (Titrant volume in step 9)

SV= [(Vb-Vs)x Normality of KOH x equivalent wt. of KOH)]/w

Normality of KOH = 0.5
equivalent wt. of KOH =56.1
w= Oil sample weight (g)

Result :-

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 10

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Experiment No.: 5

Aim: - To prepare detergent in the laboratory and to carry out its cost analysis.

Apparatus: - Beaker, Wooden tray, Weighing scale, etc.

Chemicals: - Acid slurry, Soda ash, Urea, Carboxymethyl cellulose, Tripolyphosphate, Common
salts.

Theory: -

Development of synthetic detergent is a big achievement in the field of cleansing.

They can be used with hard water as well and also in acidic solution. These are salts of
sulphuric acids or alkyl hydrogen sulfates.

A detergent is a formulation comparing essential constituents (surface active agents) and

subsidiary constituents (builders, boosters, filters and auxiliaries.)

The various ingredients of detergents are:

Ingredients Function

1. Surfactants (Surface active agent) Removal of oily soil, cleaning

2. Buliders
(a) Sodium tripolyphosphate Removal of inorganic soil, detergent building.
(b) Sodium sulfate Filler with building action in soft water
(c) Soda ash Filler with some building action
3. Additives
(a) Sodium silicate Corrosion inhibitor with slight building action
(b) Carboxy Methyl Cellulose Attire deposition of soil
(c) Fluorescent dyes Optical brightening
(d) Tarnish inhibitors Prevention of silverware tarnish
(e) Perfume Aesthetic, improved product characteristic
(f) Water Filler and Binder

Procedure: -

1. Take the entire chemical in their proportional weight.

2. On a tray, crush the lumps of soda ash to a fine powder.
Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 11
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3. Add the acid slurry to the powder slowly and mix thoroughly with hand.
4. Add trisodium phosphate, urea, carboxy methyl cellulose, salt in the given proportion.
Material Weight %
Acid slurry 18
Soda ash 70
Tripoly phosphate 2
Urea 4
Carboxy methyl cellulose (CMC) 2
Salt 2

Observations:

Material Used Cost Rs./Kg Quantity used (gm) Cost of material

(approx)
Acid slurry 140
Soda ash 50
Tripoly phosphate 600
Urea 180
Carboxy methyl 5
cellulose (CMC)

Calculations: -

1. Packing Charge: 0.50 Rs.

2. Total cost Rs. : --------------------.

Result:

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 12

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Experiment No.: 6

Aim:- To determine the acid value of given oil sample.

Principle:-
Neutralization number refers to the determination of the acidic or basic constituents of oil.
Determination of acidic constituents is more common and called acid number or acid value.

The acid value of oil is the number of milligrams of potassium hydroxide required to neutralize
the free acids present in 1 gm of the oil sample. The presence of mineral acids in oil is so rare that
is almost unnecessary to look for it. In good oils, the acid value should be very low (< 0.1). The
acid value greater than 0.1 should be taken as an indicator for oxidation of oil which may lead to
form gum and sludge. The acid value of fatty oils may vary from 0.2 to 50 and it shows the extent
of hydrolysis of glyceryl ester of the oil. Acid value of oil can be determined by dissolving a
known weight of sample in a suitable solvent and titrated it with a standard solution of KOH to
definite end point.

H+ + OH- ↔ H2O
RCOOH + KOH ↔ RCOOK + H2O

Apparatus:-
Conical flask, burette, pipette, water bath

Reagents:-
N/10 alcoholic KOH, Neutral Methanol, phenolphthalein indicator.

Procedure:-
1. Weigh about 5gm of sample oil in 250ml conical flask.
2. Add 50 ml of neutral alcohol in flask. Stir well to dissolve the oil.
3. Add few drops of phenolphthalein indicator in the flask.
4. Titrate the analyst with standard N/10 alcoholic KOH solution until a faint permanent
pink color appears at the end point.
5. Note the volume of N/10 KOH solution consumed during titration.
6. Repeat the same procedure for another oil sample.

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Note: sometimes the pink color at the end point may fade away after a little while due to the
attack of alkali upon some easily reactable materials in the oil, particularly when the mixture is
violently shaken. In such cases, the titration should be done rapidly and the first end point should
be considered.

Observation:-
Burette: N/10 standard KOH
Conical flask: Oil + 50 ml neutral Alcohol
Indicator: Phenolphthalein
Colour Change: Colourless to light pink

Sample 1:
Initial weight of 250 ml conical flask: ……………..gms
Wt. of conical flask + oil: ……………..gms
Wt. of oil: ……………………gms
Volume of N/10 KOH used in titration: …………….ml

Calculation:-

Acid Value = Burette reading x Normality of KOH x equivalent weight of KOH

Wt of oil
Acid Value = Burette reading x 0.1 x 56.1
Wt of oil

Where, 5.61 represent the amount of KOH in mg present per each ml of N/10 KOH solution.
(1000 ml of 1 N KOH ≡ 56.1 gm of KOH)

Result :- The acid value of given oil samples of oil is (1)…………………………………

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 14

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Experiment No.: 7

Aim: Synthesis of Biodiesel from vegetable oil

Apparatus: 250 ml Beaker, Measuring Cylinder, Separating funnel

Chemicals/ Reagent : Vegetable oil, Methanol, KOH / NaOH, Distilled water.

Theory :

Biodiesel, a methyl ester, is an alternative to diesel that is made from a triglyceride (like vegetable
oil) and either ethanol or methanol. The oil used in the process can come from many sources
including soybeans, corn, canola, and used frying oil. Because it comes from renewable resource,
it is referred to as a biofuel. The process involves taking the oil, a triglyceride, combining it with
an alcohol, to form biodiesel, which is either an ethyl ester or a methyl ester. The process uses a
base, either potassium hydroxide or sodium hydroxide, as a catalyst to help in the process and
forms glycerol as a byproduct. The reaction is shown below:

The process involves combining the methanol with the catalyst, in this case sodium hydroxide.
This forms sodium methoxide, very strong base which is then combined with the vegetable oil.
After the reaction is complete, the oil and glycerol form two separate phases with the glycerol
being on the bottom and the biodiesel on the top. The glycerol is then removed and the biodiesel
layer is then rinsed with water to remove any remaining catalyst. In today’s lab, we will be
making biodiesel on a small batch scale. The usual biodiesel process is a continuous process that
involves large tanks and pumps. This lab will give you an idea of what happens inside the vessels
and pipes as biodiesel is being made.

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Procedure:

1. Take a 50 mL Erlenmeyer flask with a stir bar and add 14 ml of pure methanol.
2. Place the flask on a stir plate and set speed at a rate where it doesn’t splash but stirs
vigorously.
3. Slowly add 0.50 g of NaOH. Do not go over this mass of the NaOH; add carefully.
4. Observe the NaOH being completely dissolved. Once this happens, sodium methoxide is
formed, a very strong and dangerous base.
5. While the sodium methoxide is being formed, place 60 ml of pure vegetable oil in a 200
ml beaker on a hot plate and warm to 50°C. Then place it on a stir plate with a stir bar
under medium agitation.
6. After step 4 is complete, SLOWLY the sodium methoxide add it to the warm vegetable
oil. Make sure no residual NaOH gets into the oil. The solution will be cloudy.
7. Stir the reaction mixture for 20 minutes
8. Transfer the solution to a 125 ml separatory funnel. Allow the solution to settle for 20
minutes using a ring stand; the glycerol layer will form on the bottom. If you do not see
two layers, start over being sure to add no more than 0.50 g NaOH.
9. Once glycerol has stopped forming, drain the glycerol into a small graduated cylinder
using the stopcock. Record the volume of glycerol.
10. Drain the biodiesel layer from the separatory funnel and measure the volume

Calculation:

Result:

Conclusion :

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 16

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Experiment No.: 8

Aim: - To prepare Acetanilide from Aniline.

Theory:-

Acetanilide is an odourless solid chemical of leaf or flake-like appearance. It is also known as N-

phenylacetamide, acetanil, or acetanilid, and was formerly known by the trade name Antifebrin.
Acetanilide is slightly soluble in water, and stable under most conditions. Pure crystals are plate
shaped and colorless to white.

Acetanilide is used as an inhibitor in hydrogen peroxide and is used to stabilize cellulose ester
varnishes. It has also found uses in the intermediation in rubber accelerator synthesis, dyes and
dye intermediate synthesis, and camphor synthesis. Acetanilide is used for the production of 4-
acetamidobenzenesulfonyl chloride, a key intermediate for the manufacture of the sulfa drugs. It
is also a precursor in the synthesis of penicillin and other pharmaceuticals.

Reaction: - Acetanilide can be produced by reacting acetic anhydride with aniline:

C6H5NH2 + (CH3CO)2O → C6H5NHCOCH3 + CH3COOH

Apparatus: - Conical flask, funnel, filter papers, sand-bath, etc.

Chemicals: - Acetic acid, Acetic anhydride, Conc. H2SO4, Ice, etc.

Procedure: -

Take about 5 ml of aniline in a small dry conical flask. To it add 10 ml of mixture of acetic
acid and acetic anhydride and 1 to 2 drops of conc. H2SO4 heat the mixture gently for 5 to
10 minutes keeping a funnel over the conical flask on a sand-bath. Pour the hot liquid in
ice cold water, stir it well, filter the product and wash it with cold water. Recrystallize it
from hot water, M.P. 113oC.

Result: -

Acetanilide obtained = _____.

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 17

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Experiment No.:9

Aim: - To prepare m-dinitrobenzene from Nitrobenzene.

Theory:-

Dinitrobenzenes are chemical compounds composed of a benzene ring and two nitro group
(-NO2) substituents. The three possible arrangements of the nitro groups afford three isomers, 1,2-
dinitrobenzene, 1,3-dinitrobenzene, and 1,4-dinitrobenzene. Each isomer has the chemical
formula C6H4N2O4 and a molar mass of about 168.11 g/mol. 1,3-Dinitrobenzene is the most
common isomer and it is used in the manufacture of explosives.

Reaction: - 1,3-Dinitrobenzene is accessible by nitration of nitrobenzene. The reaction proceeds

under acid catalysis using sulfuric acid. The directing effect of the nitro group of nitrobenzene
leads to 93% of the product resulting from nitration at the meta-position. The ortho- and para-
products occur in only 6% and 1%, respectively.

Apparatus: - Conical flask, Funnel, Stirrer, Sand-bath, Filter papers, etc.

Chemicals: - Nitrobenzene, Conc. HNO3, Conc. H2SO4, Ice, etc.

Procedure: -

Take 25 ml of nitrating mixture (containing 10 ml of conc. HNO3 and 15 ml conc.

H2SO4) in a conical flask, and then add 5 ml Nitrobenzene slowly from funnel. Stir the
mixture well and heat it on a sand-bath till complete evolution of brown fumes (for about
10 min.). Test the portion of a mixture by adding in ice cold water. If the solid separates,
add whole mixture slowly over ice, stir well and filter. Wash the product with water and
recrystallize it from rectified spirit (or hot water)

Result: -

m-dinitrobenzene obtained = _____.

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 18

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Experiment No.:10

Aim: - To prepare Benzoic acid from Toluene.

Apparatus: - Round bottom flask, Reflux condenser, Wire gauze, Stirrer,

Filter papers, Porcelain, etc.

Chemicals: - Toluene, Na2CO3, KMnO4, Conc. HCl, Ice, etc.

Reaction: -

Procedure: -

Take 5.0 gm of Toluene in a round bottom flask contained about 100 ml of water.
Attach the reflux condenser to the flask, add pieces of porcelain. Also add 3.0 gm of
Na2CO3. Heat the reaction mixture on wire gauze and add 8.0 gm of KMnO4 gradually
with constant stirring. Reflux the flask by heating till violet colour of permanganate
disappears. Remove unoxidixed toluene by steam distillation. Filter the reaction mixture to
remove manganese dioxide wash twice with water. Acidify the filtrate with conc. HCl, on
cooling benzoic acid separates out. Filter the cold solution, wash with cold water and dry
the acid. Recrystallize from hot water. M.P. 121oC.

Result: -

Benzoic acid obtained = _____.

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 19

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Experiment No.: 11

Aim: - To prepare Anthraquinone from Anthrancene.

Apparatus: - Conical flask, sand-bath, Filter papers, etc.

Chemicals: - Anthrancene, Conc. HNO3, Ice, etc.

Reaction: -

Procedure: -

1. Take about 1 gm of Anthracene in dry conical flask.

2. Add 10 to 15 ml of conc. HNO3 and heat the flask gently on sand-bath till the
brown fumes are completely removed (for about 15 min.).
3. Then pour the mixture in ice cold water, filter it and wash with water and dry
it. M.P. 286oC.

Result: -

Anthraquinone obtained = _____.

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 20

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Experiment No.: 12

Aim: - To prepare sulphanilic acid from aniline.

Chemicals: - Aniline, Conc. H2SO4, 2 N NaOH solution, Oil bath, Ice, etc.

Procedure: -

In a flask take 10 ml of aniline and add 20 ml of concentrated sulfuric acid in small

proportions with stirring and cooling the flask occasionally in an ice bath. Reflux the
reaction mixture in oil bath between 180 – 190 C for five six hours when the sulphonation
will be completed (test portion of solution will be dissolved completely without leaving
any free aniline in 2 N NaOH) cool the product and pour the solution with shaking to
water having enough crushed ice in a beaker. Allow the product to stand for 10 minutes,
filter it and then wash it with ice-cold water and dry. Recrystalline the crude sulphanilic
acid from boiling water.

Result: -

Sulphanilic acid obtained = _____.

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 21

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Experiment No: 13

Aim: To Prepare Salicylic Acid From Methyl Salicylate.

Apparatus Required:
➢ Round bottom flask
➢ Heating mantle
➢ Water reflux condenser
➢ Thermometer
➢ Water bath
➢ Beakers
➢ Measuring cylinder

Chemicals Required:
➢ Methyl salicylate
➢ Concentrated hydrochloric acid
➢ 20 % w/w Sodium Hydroxide

Reaction
COOCH3 COONa COOH

OH OH OH
+ NaOH HCl OH
-CH3OH

Methyl Salicylate Sodium Salicylate Salicylic Acid

Theory:
Salicylic acid is prepared from methyl salicylate. Methyl salicylate is reacted with Sodium
Hydroxide and finally is acidified with hydrochloric acid to convert into salicylic acid.

Procedure:
➢ 10 ml. of methyl salicylate and 10 ml. of w/w sodium hydroxide solutions are taken in a small
round bottom flask. Small pieces of glass or porcelain are also taken in the flask to withstand
over heating.
➢ Then water reflux condenser is joined to the round bottom flask. The whole mixture in the
round bottom flask is gently heated in water bath continuous reflux for about 30 min.
➢ After refluxing for 30 min. reflux condenser is removed and the flask is cooled. Then the
contents are transferred in to a beaker.
➢ Afterwards concentrated hydrochloric acid is added slowly with continuous stirring to acidify
the solution. Final condition is predicted by checking its pH using litmus paper. The content is
cooled under tap water. The cooled product is collected in the paper is taken in glass funnel.
The product is washed with water over this filter paper and it is dried.
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➢ The dried product is accurately weighed and is noted as final; product weight in the
observation table.

Observation:
➢ Final weight of Salicylic acid dried = gm.
➢ Volume of Methyl Salicylate taken = ml.
➢ Density of Methyl Salicylate = 1.184 gm/ml
➢ Weight of Methyl Salicylate taken = gm.

Calculation:
➢ Molecular weight of Methyl Salicylate = 152.15 gm/gmol
➢ Molecular weight of Salicylic Acid = 138.12 gm/gmol
➢ Theoretical Yield is calculated as below from the reaction as

Reaction
COOCH3 COONa COOH

OH OH OH
+ NaOH HCl OH
-CH3OH

Methyl Salicylate Sodium Salicylate Salicylic Acid

152.15 gm. of Methyl Salicylate is required to produce 138.12 gm. of Salicylic Acid.

 1.184 gm. of Methyl Salicylate is required to produce Salicylic acid

= (1.184 * 138.12) / 152.15

= gm

= i.e. Theoretical Yield

➢ Practical Yield = Final weight dried Salicylic Acid = gms.

➢ Percentage Yield =  Practical Yield / Theoretical Yield  * 100 = %

Result:

Percentage yield of Salicylic Acid = %

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 23

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Experiment No: 14

Analysis Of Sulfa Drug

Aim: To find the purity of sulfa drug.

Theory:
➢ In medical line, to perform the analysis of various Sulfa drugs is of prime interest.
➢ There are many example of the sulfa drug such as Sulfa pyridine, Sulfa dyagin, Sulfa thiazol
and sulfa marazine.
➢ They have one characteristic to give insoluble precipitates with silver nitrate solution.
➢ Their purity is measured by dissolving it in the mixture of acetone and sodium acetate with the
use of potassium dichromate as indicator. Afterwards the dissolved mixture is titrated against
standardized silver nitrate solution.
➢ In other way, precipitation is done in more amount of silver nitrate solution to get the silver
salt. This silver salt is filtered and is dried. Its purity is found out based on gravimetric
analysis.

Apparatus:
➢ Beaker 500 ml. and 1000 ml.
➢ Conical flask 250 ml.
➢ Measuring cylinder 100 ml. and 10 ml.
➢ Burette & Pipette
➢ Water bath

Chemicals:
➢ 0.1 N Silver Nitrate solution
17 gm. Silver Nitrate is dissolved in 1 liter of distilled water.
➢ 0.1 N Ammonium Thiocyanate solution
7.6 gm. Ammonium Thiocyanate is dissolved in 250 ml. of distilled water. Dilute the
solution up to 1-liter volume using distilled water.
➢ 10% w/w Sodium acetate solution
20 gm. Sodium acetate is dissolved in 200 ml. distilled water.
➢ 10% v/v Nitric Acid solution
20 ml. concentrated nitric acid is dissolved in 200 ml. distilled water.
➢ 0.5% w/w Sodium Dichromate solution (indicator)
0.5 gm Sodium Dichromate is dissolved in 100 ml. of distilled water.
➢ 10% w/w Ferric Ammonium Sulphate solution
10 gm Ferric Ammonium Sulphate is dissolved in 100 ml. of distilled water.
➢ Acetone

Procedure:
Sample titration
➢ 0.2 gm. of sulpha medicine (e.g. Sulfa pyridine, Sulpha dyajol or Sulfa thiajol) is accurately
weighed.

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➢ Accurately weighed sample is taken in 250 ml. of conical flask. 25 ml. of Acetone and 20 ml.
of 10% Sodium Acetate solution are taken in the same flask. Whole flask content is shaken till
it become uniform solution.
➢ Note: If required solution is heated to make completely uniform solution.
➢ 1 ml. of 0.5% Sodium Dichromate solution (as indicator) is added.
➢ The whole solution of the flask is titrated against 0.1 N Silver Nitrate solution. At the end
point the yellow color of the solution is turned to permanent red color. Final burette reading is
noted as V1.
Blank titration
➢ 25 ml. of Acetone and 20 ml. of 10% Sodium Acetate solution is taken in the 250 ml. of
conical flask. 1 ml. of Sodium Dichromate solution is added as indicator.
➢ Afterwards, the whole content is titrated against 0.1 N Silver Nitrate solution. Finally the
yellow color changed to permanent red color. This final end point is noted as V2.

Observations:
➢ Burette reading for sample titration (V1) = ml.
➢ Burette reading for blank titration (V2) = ml.
➢ Normality of Silver Nitrate solution (N1) =
➢ Molecular Weight of sulfa drug (M) =
➢ Weight of sulfa drug (W) =

Calculations:
Purity of sulfa drug is found out using below equation,
Substitute the required values from the observations
Purity of Sulfa drug = [(V1 - V2) * N1 * M * 100]/ (W * 1000)

Result: Purity of Sulfa drug =_______ %

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 25

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Experiment No: 15

Aim: To prepare Phenylazo-2-Napthol

Theory:
➢ Azo compounds (ArN=NAr) are prepared by the interaction of a diazonium salt with phenol
in the present of Sodium Hydroxide, for example

NaNO2 NaOH
C6H5NH2 C6H5N2Cl + C10H8O C6H5N=N (C10H8O) + HCl
HCl
Aniline Diazonium 2-napthol Phenylazo-2-napthol
Chloride

Apparatus:
➢ Round bottom flask
➢ Heating mantle
➢ Stirrer assembly
➢ Thermometer
➢ Water bath
➢ Condenser
➢ Beakers & Measuring cylinder
➢ Ice

Chemicals:
➢ Aniline
➢ Hydrochloric acid
➢ Sodium Nitrite
➢ 2-Napthol
➢ Sodium hydroxide
➢ Methylated spirit or methanol

Procedure:

NaNO2 NaOH
C6H5NH2 C6H5N2Cl + C10H8O C6H5N=N (C10H8O) + HCl
HCl
Aniline Diazonium 2-napthol Phenylazo-2-napthol
Chloride

Diazotization:
➢ Dissolve 5 gm of aniline in 60 ml of concentrated HCl and water (in equal proportion to HCl)
in a 250 ml beaker.
➢ Diazotize by the addition of 4 gm of Sodium Nitrate dissolved in 20 ml of distilled water.

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Coupling:
➢ Prepare a solution of 7.5 gms of 2-napthol in 45 ml of 10% NaOH solution. Cool the solution
to 50C by immersing it in ice bath assisted by direct addition of 50 gms of ice.
➢ Stir the napthol solution vigorously and add the cold diazonium salt solution slowly to it and a
red color develops giving red crystals of phenyl azo-2-napthol, which separates out very soon.
➢ When all the diazonium salt is added allow the mixture to cool in ice bath for about 30 min.
with occasional stirring.

Isolation:
➢ Filter it through the funnel & wash well with water and drain thoroughly by pressing the
crystals with back of beaker. Wash the crystallized product with little alcohol and dry upon
filter paper.

Observation:
Final weight of the dry phenylazo-2-napthol obtained = gms

Calculations:
Find the theoretical yield
NaNO2 NaOH
C6H5NH2 C6H5N2Cl + C10H8O C6H5N=N (C10H8O) + HCl
HCl
Aniline Diazonium 2-napthol Phenylazo-2-napthol
Chloride
(93 gms) (248 gms)

To produce 248 gms of phenylazo-2-napthol 93 gms of aniline is used. Therefore from 5 gms of
aniline X gms of Phenylazo-2-napthol

Theoretical yield = X gms = (5 * 248)/93 =

Practical yield obtained = Y gms =

➢ % Yield = (Practical yield / Theoretical yield)

= (Y/X) 100

Result:

The percentage yield of Phenylazo-2-Naphthol=_______%

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 27

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Experiment No.: 16

Aim: To determine the amount of potassium in the given sample of fertilizer.

Chemical: 10% sodium cobaltinitrile, 0.01M HNO3 solutions and 95% alcohol.

Theory: Potassium Fertilizers inorganic substances used as a source of potassium nutrition for
plants; usually salts of hydrochloric, sulfuric, and carbonic acids dissolved in water—often
combined with other compounds containing potassium—in a form accessible to plants.
Potassium fertilizers are divided into raw potassium salts, which are produced by mechanical
processing (sorting, crushing, and pulverization) of natural potassium salts, and concentrated, or
high-analysis, potassium fertilizers, such as potassium chloride, potassium sulfate, and 30-percent
and 40-percent potassium salts (a mixture of finely ground natural kainite or sylvinite with
potassium chloride), as well as potash, potassium-magnesium sulfate, potassium electrolyte, and
ash

Process: Dissolve 1 gm of the KCl in the small quantity of dis.water in a 250 ml beaker. Add 1 ml
of dil. HNO3 acid. Dilute the prepared solution to 250 ml by addition of dis.water in measuring
flask. Pipette out 50 ml this solution in a clean and dry 250 ml beaker. Add 25 ml of 10% sodium
cobaltinitrile.mix and allow standing for two hours. Filter the content by what man filter paper
[weighed].transfer the precipitate using 2 ml alcohol.repaet the similar alcohol washing at least for
five tomes.dry the precipitate for 1 hr. at 110oc in air oven. Cool and weigh it. Express the weight
as amount of K in sodium cobaltinitrile.

Calculation:
1gm sodium cobaltinitrile = 0.1722gm of potassium
So W gm = W X0.1722 gm of potassium in 50 ml diluted solution.
= W X0.1722 gm of potassium in 250 ml
= Y gm of potassium
So % potassium = Y gm x 100

Result: Percentage of potassium in the given sample=………..%

Questions:
1. State the need for fertilizer analysis.
2. What do you understand by NPK fertilizer?
3. State the drawbacks of using excess fertilizer.
4. State the types of fertilizers.
Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 28
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5. What are nutrients? State the essential nutrients for plants.

Experiment No.: 17

Total insoluble residue in cement

Aim: To determine the total insoluble residue in the cement sample.

Requirement: sample, evaporating dish , conc.HCl, 10% NaOH solution, methyl red indicator,
conical flask,funnel,2% NH4Cl,crucible, ash less filter paper.

Process: Weigh 1 gm of sample in evaporating dish; add 10 ml dis.water and 5 ml conc.HCl then
heat till no more effervescence are given out. Add 40 ml dis.water and digest on a steam bath for
15 min. filter this in filter paper and wash it hot dis.water.dossolve the residue in 100 ml 10%
Noah solution .acidify the solution with conc.HCl using methyl orange indicator and add a few
drops of acid in excess. Filter it with ash less filter paper and wash with 2%NH4Cl solution. Dry
and ignite the filter paper with residue in desiccators and weigh. Heat again, cool and find
constant weight. Note down the observation.

Calculation: % total insoluble residue = W2/ W1 X 100

Where: W1 is initial weight of sample
W2 is weight of residue

Results: Total insoluble residue in the sample is …………. %

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 29

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Experiment No.: 18

Fertilizer analysis

Aim: To determine the amount of calcium in the given sample of fertilizer volumetrically.

Apparatus: Burette, pipette, conical flask, beaker

Chemicals: Ca precipitating buffer solution, dil.H2SO4, 0.01M KMnO4, 2M H2SO4.

Process: Take 100 ml of the given sample solution into 250 ml beaker. Add 30 ml of Ca
precipitating buffer solution to the content of the beaker. Stirrer and allow to stand for 1 and half
hour. Filter the precipitates in dil.H2SO4 acid solution and make the volume to 250 ml using
dis.water in a measuring flask. Pipette out 25 ml of diluted solution in a clean and dry conical
flask add 25 ml 2 M H2SO4 acid solution. Heat and titrate it against 0.01M KMnO4 solution till
permanent pink color is obtained.

Calculation:
CaCl2 + (NH4)2C2O4 ……….CaC2O4 + 2NH4Cl
CaC2O4 + H2SO4……………CaSO4 + H2C2O4
2 KMnO4 +3 H2SO4………….K2SO4 + 2MnSO4 + 3H2O +6O
5 H2C2O4 + 5O……………5H2O + 10 CO2
From the equation: 2 KMnO4 = 5 mole of H2C2O4 = 5 mole of CaC2O4
Moles of KMnO4 = Z X 0.01/1000 = Z X 10-3 moles = Y
1 ml 0.01M KMnO4 = 0.40 gm Ca
Z ml of 0.01 KMnO4 = Z X 0.40gm Ca
Y moles of KMnO4 =
Amount of Ca present in diluted solution = moles x mol.wt.
= Y X 40
Amount of Ca in the given solution = Y X 40 X 10 =…………

Results: Amount of Ca in the given sample solution = ………..

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 30

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Experiment No.:19

Analysis of Na2CO3 and NaHCO3 mixture

Aim: To determine the amount of Na2CO3 and NaHCO3 in the given mixture of sodium carbonate
and sodium bicarbonate.

Apparatus: Burette, pipette, conical flask, beaker

Theory: The determination of strength of Na2CO3 and NaHCO3 present in solution is based on
selective use of indicators
When methyl orange is used as an indicator, the volume of 0.1 N HCl in the titration will
neutralize both, Na2CO3 andNaHCO3 completely.
Na2CO3 + 2HCl………….2NaCl + H2O
NaHCO3 + HCl ………….NaCl +H2O + CO2
Let the volume of acid used in x ml when methyl orange is used as indicator.
When phenolphthalein is used as indicator the volume of 0.1 N HCl used in titration will
correspond half neutralization of Na2CO3 up to half stage.
NaHCO3 + HCl ………….NaHCO3 + NaCl
Let the volume of acid for neutralization is Y ml when phenolphthalein is used as indicator. In
fact it does not give color in NaHCO3 solution.
There for the volume of acid used for complete neutralization Na2CO3 will be 2Yml and volume
of the acid used for neutralization of NaHCO3 will be X- 2Y
Therefore two different titration are carried out with the given mixture using methyl orange and
phenolphthalein indicator respectively.

Process:
1. Rinse and fill the burette with 0.1NHCl
2. Pipette out 10 ml alkali mixture solution into conical flask. to it add 2—3 ml methyl
orange
3. Run HCl into the flask till the yellow color of the solution changes to red. let the volume
of the acid used is X ml.

Using phenolphthalein as indicator

1. Pipette out 10 ml of alkali mixture solution into conical flask.
2. To it add 2-3 ml of phenolphtheline.run 0.1 N HCl from the burette into the flask till the
pink color of the solution changes to colourless.let the volume of the acid used Y ml.

Observation: 1. Volume of titrant used………..ml

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 31

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Observation: 2. Volume of titrant used………..ml

Calculation: volume of acid required for neutralization Na2CO3 up to half stage = Y ml

So volume of acid required for neutralization Na2CO3 completely = 2y ml

N1V1 = N2V2
N2=…………

Hence the strength of Na2CO3 In the solution = Normality x Eq.wt. =………

Volume of acid required for complete neutralization Na2CO3and NaHCO3 present in the
mixture = X ml
So volume of acid required for neutralization of NaHCO3 only =(x-2y) ml
N1V1 = N2V2
N2 = 0.1 X (X-2Y) / 10 = (X-2Y)/ 100
Hence the strength of NaHCO3 in the solution = normality x eq.wt.
= (X-2Y) X 84 / 100

Result: The amount of Na2CO3 present in the given mixture = ………….gm/l

The amount of NaHCO3 present in the given mixture = ………….gm/l

Questions:
1. State the need for the analysis of Na2CO3 andNaHCO3 in the given mixture.
2. State the different methods of analyzing mixtures.
3. State applications of Na2CO3 andNaHCO3.

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 32

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Experiment No.: 20

Analysis of bleaching powder

Aim: Determination of percentage available chlorine in bleaching powder.

Apparatus: burette, pipette, conical flask, beaker

Principle:

Most hypochlorites are normally obtained only in solution, but calcium hypochlorite exists in the
solid form in commercial bleaching powder which consists essentially of a mixture of calcium
hypochlorite Ca(OCl)2 and the basic chloride CaCl2,Ca(OH)2,H2O; some free slaked lime is
usually present. The active constituent is the hypochlorite, which is responsible for the bleaching
action. Upon treating bleaching powder with hydrochloric acid, chlorine is liberated:

ClO- +C1- + 2H+ = C12 + H2O

The available chlorine refers to the chlorine liberated by the action of dilute acids on the
hypochlorite, and is expressed as the percentage by weight in the case of bleaching powder.
Commercial bleaching powder contains 36-38 per cent of available chlorine.

Two methods are in common use for the determination of the available chlorine. In the first, the
hypochlorite solution or suspension is treated with an excess of a solution of potassium iodide,
and strongly acidified with acetic acid:

ClO- + 2I- + 2H+ = Cl- + I2 + H2O

The liberated iodine is titrated with standard sodium thiosulphate solution. The solution should
not be strongly acidified with hydrochloric acid, for the little calcium chlorate which is usually
present, by virtue of the decomposition of the hypochlorite, will react slowly with the potassium
iodide and liberate iodine:

I2 + 2S2O3 ………..2I + S4O6

Process:

1. Fill the burette with Na2S2O3 solution

2. Pipette out 25 ml of bleaching powder solution in a conical flask
3. Add 25 ml dis.water,followed by 1-2 gm of solid KI and 10 ml of glacial acetic acid

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 33

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4. Keep the solution in dark for 3-4 min.

5. Titrate the solution with Na2S2O3 solution till the brown color change to pale yellow
6. Add 1-2 ml starch, the solution will turn blue
7. Continue the titration till the blue color disappears
8. Repeat the same for constant.

Observation: Normality of Na2S2O3 solution N1 = 0.1 N

Observation table:

Volume of the titrant used V2 =…………..

Calculation:

N1V1 = N2V2

N1 = I/10 X V2/25

(Z) Amount of Cl2 = N1 X EQ.WT.

% Available chlorine = [ (Z x 250 /1000)/W] X100 =……..

Where W is the weight of bleaching powder dissolved in 250 ml dis.water for preparing the
solution of bleaching powder.

Result: The available chlorine in the given sample =…………. %

Questions:

1. State the merits and the demerits of using bleaching powder for disinfection purpose.
2. What are the advantages of using bleaching powder over other disinfectants?
3. State the drawbacks of excess chlorine in drinking water.

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 34

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Experiment No:21
Proximate analysis of Coal

Aim: To study the proximate analysis of given coal sample.

Theory:
➢ Coal is coming in various qualities. 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 applications 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.
➢ Proximate analysis
➢ Ultimate analysis
➢ Proximate analysis is the simplest way of analyzing the coal. The following contents are found
in analysis.
• Fixed Carbon
• Volatile Matter
• Moisture
• Ash (Mineral Matter)

➢ Ultimate analysis is the specific method of analyzing the coal. The following contents are
found out.
• Carbon
• Hydrogen
• Nitrogen
• Oxygen
• Sulphur
• Its Heating Value

Apparatus Required:
➢ Muffle Furnace
➢ 200 mesh size sieve
➢ Weighing Balance

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 35

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➢ Silica Crucible with air tight lid

Asbestos hand gloves

➢ Desiccators
➢ Pair of tongs

Procedure:
➢ First small pieces of coal were crushed and are passed through 200 mesh size sieve.
➢ From the under flow of the sieve, accurately weighed 2 gm of sample in the crucible and a lid
is weighed and total weight is noted
➢ Moisture Content
➢ Crucible is kept in furnace and temperature in the furnace is raised up to 110 0 C. to remove
the moisture.
➢ Now the crucible is taken out carefully and is kept in the desiccators with CaCl2 to cool down
up to room temp. Then whole crucible is weighed again and weight is noted down.
➢ The weighed crucible is kept again in the furnace.
➢ Volatile Matter
➢ Now, temp. in the furnace is raised up to 900 0 C. and temp. is kept constant for 7 minutes to
remove the volatile matter.
➢ Crucible is taken out and is kept in the desiccators to cool down up to room temp. Crucible is
again weighed and note down the weight.
➢ Ash content
➢ Lid over the crucible is removed and is heated from 5000 C. to 815 0 C. for 1 hrs.
➢ Again the crucible is kept in the desiccators to cool down up to room temp.
➢ This crucible is weighed and weight is noted
Observations:
➢ Weight of the empty crucible = a gm. =
➢ Weight of a lid = b gm.=
➢ Weight of the crucible sample = c gm. =
➢ Weight of the crucible after heating up to 1100 C. = d gm. =
➢ Weight of the crucible after heating up to 9000 C. e gm. =
➢ Weight of the crucible after heating up to 8150 C. = f gm. =

Calculations:
➢ Weight of crucible with sample and the lid = a+b+c gm. = w gm.
➢ Weight of moisture gone out = (w-d) gm. =

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➢ Weight of the volatile matter gone out = (d-e) gm. =

➢ Weight of the ash remaining after the final heating = f- (a+b) gm. =
➢ Moisture fraction in the sample = (w-d)/c = x* 100 =
➢ Volatile Matter fraction in the sample = (d-e)/c =y* 100 =
➢ Ash fraction in the sample = (f- (a+b))/c = z* 100 =
➢ Fixed carbon fraction in the sample = (1- (x+y+z))* 100 =

Result:
Proximate analysis of the given coal sample:
Moisture percent =
Volatile Matter percent =
Ash percent =
Fixed Carbon percent =

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 37

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Experiment No.: 22

Determination of the Sodium Carbonate in the Washing Soda

Aim: To determine the sodium carbonate content in the washing soda.

Apparatus Required:
➢ Weighing Balance
➢ Measuring Cylinder (1liter, 500 ml and 10 ml)
➢ Burette (50 ml)
➢ Graduated Pipette (25 ml)
➢ Conical Flask (250 ml)

Chemicals Required:
➢ Washing Soda-crystals
➢ 0.1 M Hydrochloric acid solution: 9 ml of concentrated Hydrochloric Acid is taken in 1 liter
of measuring cylinder and dissolved by 500 ml. of distilled water. At last it is diluted up to 1-
liter quantity using distilled water. It is thoroughly mixed.
➢ Methyl orange-Indigo Carmine Indicator / Bromocresol green indicator.

Theory:
Washing soda is mainly consisting of Sodium Carbonate. It is used in washing clothes and is also
used for other domestic purpose. It enhances the cleaning action during washing.

Procedure:
➢ 3.6 gm. of Washing Soda crystals is accurately weighed. It is dissolved in 100 ml. of distilled
water in measuring cylinder (500 ml.) and is diluted up to 250 ml. using distilled water and is
mixed thoroughly.
➢ 25 ml. of Washing soda solution is taken in 250 ml. of conical flask. Burette is filled with std.
0.1 M Hydrochloric solution. Then Washing Soda solution is titrated against 0.1 M
Hydrochloric solution by adding 2 drops of Bromocresol Green as indicator.
➢ The final end point is found out by color change and the final burette reading is noted as V 1
ml.

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Observations:
➢ Weight of Washing Soda is taken (W3) = gm
➢ Final Burette reading (V1) = ml
➢ Molarity of HCl used in burette (M) =

Calculations:
Weight of anhydrous Sodium Carbonate Na2Co3, which, has reacted with the standard HCl
solution can be readily calculated from known weight of washing soda.

Na2CO3 + 2HCl 2NaCl + H2 O + CO2

106 2(36.5) (58.5) 18 44

1 ml of 1 N HCl = 0.053 gm .of Na2CO3

x ml of 1 N HCl =(?) gm of Na2CO3

Weight of Washing Soda in portion titrated = W3 * 25.0/250

= A gm

Percentage of Na2CO3 = (z * 100) /A =

Result:Percentage of Sodium Carbonate in Washing Soda = %.

Conclusion:

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 39

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Experiment No.: 23

Analysis of cement

Aim: To determine the loss on igniting the cement sample.

Requirment: Crucible, cement sample, burner etc.

Theory: Cement is technical name of a product which is considered to be a mixed silicate and
alumino-silicate.thus the constituent’s foe determination will be silica, alumina, ferric hydroxide,
lime and magnesia. In fact over 90% of the cement produced worldwide is what is known as
PORT LAND CEMENT although its use has been ubiquitous, the gelling of cement is still not
known clearly. Most molecules form in crystalline shapes where every atom has its place and this
order is usedx-rayto show the molecules are put to gother.but molecules like cement gels are
amorphous.
Process: Weigh accurately about one gram of the sample in dry, clean and previously weighed
crucible. Heat the crucible on the burner for 15 min.cool the content in desiccators and weigh
it.reoeat the exercises till constant weight is obtained. Record the observation

Calculation: % loss on ignition= W1-W2 X 100 /W1

Where
W1-Initial weight of sample.
W2is final weight of sample.

Results: The % loss on ignition is………………%

Questions:
1. State the types of cement.
2. State the basic constituents of cement.
3. What do you understand by RCC? What is its function?

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 40

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Experiment No.:24
Estimation of silica in cement

Aim: To determine the total silica in the given sample.

Requirment: solid NH4Cl conc, HCl, distilled water, beakers, funnels, wash bottle, crucible
wahtmanfilter paper no-4, etc.

Introduction:
What is Silica Cement Admixture?

Silica Cement Admixture is the finely grinded materials that bonds the concrete tighter and
enhances the strength, safety and durability of the concrete giving it high water resistance and
other advantages
Characteristics of the Silica Cement Admixture

1. Water Resistance:
• At the time of heat of hydrations of cement, the main component, Silica (Si02) produce Silica
gel layer and fills up the narrow crevices of concrete structure resulting high density concrete.
• Water resistance capability in permanently in the concrete structure.
• Single layer of concrete gives better result in sub structure like underground parking,
warehouse, Water tanks etc.

2. Prevents efflorescence:
With the mixing of the Silica Cement Admixture calcium hydroxide remains within the concrete
helps avoid the efflorescence

3. Improved durability against salt water and chemicals:

Concrete with Silica Cement Admixture is highly durable to salt water, acid and dense in mix,
reducing penetration of chloride ions and avoids corrosion of the concrete and reinforcing rod.

4. Improved Strength:
Because of the fineness of Silica Cement Admixture it fills up the whole voids between the
cement particles which enable to enhance the strength and frictional resistance.

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 41

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5. Bleeding Prevention:
After mixing the water reaction starts actively in the earlier stage and enable to bind the concrete
tightly which will absorbs excess moisture and reduces bleeding.

6. Prevention of Freezing and Melting:

With the appropriate mixing of Silica Cement Admixture in porous concrete it enable preventing,
freezing and melting of moisture within the concrete.

7. Resistance to Separation
• Silica Cement Admixture improves bonding and adhesion of the other minerals and admixture
within the concrete it provides better resistance to separation.
• With high fluidity, it facilitates the concrete placing process more smoothly.

8. Longest Expire Period

It is the product of natural Volcano Deposit so it has longest period of expiree date.

Process: Transfer the residue quantitatively to 250 ml beaker. Add 1gm NH4Cl.mix thoroughly.
add conc. HCl drop wise with constant stirring. Heat the beaker on boiling water bath for 0.5 hr.,
then add 50ml of dis.water.filter through whatmanfilter paperno-4,wash the precipitate twice with
1:7 HCl solution and then with dis.water till it is free from chloride.collecr the filtrate in 150ml
measuring flask and preserve it for the determination total oxide, lime and magnesia. Dry and
ignote the residue in a weighed crucible. Heat for 0.5hr and cool in desiccators, weigh, and heat
again for constant weight is obtained. Record your observation.
Calculation:
% total silica = W2/W1 X100
Where
W1-Initial weight of sample.
W2is weight of residue.

Results: Total silica in the sample cement is …………. %

Questions:
1. State the importance of this experiment.
2. State the applications of cement.

Chemical Engg. Dept., Pandit Deendayal Petroleum University, Gandhinagar 42