3140508 – UPCT

Chemical Engineering Department

VGEC

3140508 – Unit Process and Chemical Technology

Laboratory Manual

Chemical Engineering Department

Vishwakarma Government Engineering College

Chandkheda
 3140508 – UPCT
Chemical Engineering Department
VGEC

INDEX

Experiment List of Experiments Mapped

Nos.. COs
--- Introduction to Unit Process and Chemical Technology, Briefing about --
list of experiments with objectives, Assessment policy for experiments
1 To prepare soap in the laboratory and carry out its cost analysis
2 To prepare detergent in the laboratory and to carry out its cost analysis.
3 To determine saponification value of oil sample
4 To determine the acid value of the given sample of oil.
5 To prepare hydrated lime from the given calcium carbonate powder
6 To synthesis aspirin from salicylic acid.
7 Preparation of nitro benzene from benzene.
8 To prepare mordant yellow dye.
9 Preparation of disperse dye.
10 Preparation of fast green o dye.

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Experiment No.: …1…. Date: ………..

Soap Preparation

Objective: To prepare soap in the laboratory and carry out its cost analysis

Materials Required:
Oil, beaker , standard N/10 NaOH , glass rod, thermometer, Lard Sodium hydroxide, NaOH,
pellets Sodium chloride, NaCl, technical grade Ethanol, C2H5OH, 95% Boiling chips
Erlenmeyer flask, 125-mL Beakers, 2 400-mL, 150-mL Graduated cylinders, 25-mL, 125 or
250-mL Funnel Spatula Stirring rod Cheesecloth Ring stand Clamp to hold Erlenmeyer flask
Watch glass Scissors.

Principle:
Soaps and detergents are widely used in our society. Soaps are the product of the reaction
between a fat and sodium hydroxide:

fat + 3NaOH → glycerine + 3 soap

Soap is produced industrially in four basic steps. This article lists different steps because in
the industrial processes described each of these is done over several process steps, but in
principle it could be done in the three steps outlined here.

Step 1 - Saponification
A mixture of tallow (animal fat) and coconut oil is mixed with sodium hydroxide and
heated. The soap produced is the salt of a long chain carboxylic acid.
Step 2 - Glycerine removal
Glycerine is more valuable than soap, so most of it is removed. Some is left in the soap to
help make it soft and smooth. Soap is not very soluble in salt water, whereas glycerine is,
so salt is added to the wet soap causing it to separate out into soap and glycerine in salt
water.
Step 3 - Soap purification
Any remaining sodium hydroxide is neutralized with a weak acid such as citric acid and
two thirds of the remaining water removed.
Step 4 - Finishing
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Additives such as preservatives, colour and perfume are added and mixed in with the soap
and it is shaped into bars for sale.
Detergents are similar in structure and function to soap, and for most uses they are more
efficient than soap and so are more commonly used. In addition to the actual 'detergent'
molecule, detergents usually incorporate a variety of other ingredients that act as water
softeners, free-flowing agents etc.

Properties of soap
Emulsifying properties - Shake 5 drops of mineral oil in a test tube containing 5 mL of
water. A temporary emulsion of tiny oil droplets in water will be formed. Repeat the same
test, but this time add a small piece of the soap you prepared before shaking the test tube.
Allow both test tubes to stand for a short time. Record your observations hard water
reactions and alkalinity test - Place some soap in a 50-mL beaker containing 25 mL of
water. Warm the beaker to dissolve the soap. Pour 5 mL of the soap solution into each of
five test tubes. Add the following: Test tube 1 – 2 drops of a 5% CaCl2 solution Test tube
2 – 2 drops of a 5% MgCl2 solution Test tube 3 – 2 drops of a 5% FeCl3 solution Test tube
4 – 2 drops of tap water Test tube 5 – determine the pH of the solution using pH paper as
an alkalinity test

Procedure:
1. Measure approximately 25 g of oil into a 250-mL Erlenmeyer flask, recording the exact
mass used. Add 20 mL of ethanol and an appropriate amount of 25% (m/v) NaOH based
on the saponification value of your oil.
2. Heat the mixture in a hot water bath for about 20 min with constant, vigorous, stirring.
Keep a close watch on your flask, being prepared to lift the flask out of the water bath for
a moment if it looks as though it might be about to boil over.
3. After the odor of alcohol has disappeared and the reaction mixture is viscous with a soap-
like appearance, place the flask in an ice-water bath.
4. To precipitate out the soap, add 150 mL of a saturated sodium chloride solution to the
soap mixture while stirring vigorously. This process increases the density of the aqueous
solution, solidifies the soap and removes some excess sodium hydroxide from solution.
5. Filter the precipitated soap using vacuum filtration and wash it with two 10 mL portions of
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ice-cold water.
6. Observe and record the appearance of the soap.
7. You may choose to mold your soap or add fragrance. If so desired, gently melt your soap,
add fragrance or dye and pour into a mold. It will take at least a week for the soap to finish
drying in the mold; when dry, your instructor will return your sample.

Precautions:
1. As it is heating, some of the solution will evaporate. You must make sure that the
volume does not decrease too much, so you will need to add more liquid as the reaction
progresses. Add 5 mL portions of a mixture containing equal volumes of ethanol and
water to the beaker in order to maintain the same volume in the beaker. Also, do not let
the mixture overheat or foam over, and do not allow it to boil to dryness! If this
happens, you will need to start over.
2. Caution: the mixture of oil and ethanol will be very hot, and may splatter or catch fire.
Have a watch glass nearby to smother any flames. Wear goggles at all times, because
NaOH can cause permanent eye damage!
3. The soap may still contain NaOH, so avoid skin contact with it. Use plastic gloves if
possible.) Leave the soap to dry in your locker until the next laboratory period.
4. Ethanol is flammable. Keep the container covered and take care to avoid flames.
5. Sulfuric acid is extremely corrosive and can cause severe burns. In the event of skin
contact, immediately rinse the affected area with water. If any gets on your clothes,
remove the affected item of clothing and wash both the clothing and the area of
suspected skin contact. If skin is blistered or broken, consult qualified medical
assistance.

Cost Analysis:
Units of production = -----------

Sr. No. Particular Per unit price Total

1 DIRECT MATERIAL
2 Acids
3 Speciality chemicals
4 Ordinary chemicals
5 Perfumes
6 Direct labour
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7 Direct expense
8 Pirme Cost
Factory overheads (Fixed)
9 Depreciation
10 Rent
11 Power
12 Insurance
13 Supervisors salary
Factory overheads (variables)
14 Electricity
15 Running exp. Of machine
16 Work cost/ factory cost
Office overheads:
17 Employee cost
18 Computer
19 Telephone
21 Taxes
22 Carriage out ward
23 Cost of production
24 opening stock of finished goods
25 -Closing stock of finished goods
26 Cost of goods sold
Selling & distribution overheads:
27 Advertisement
28 Delivery vehicles
29 Petrol
30 Packaging rates
31 Cost of sales / total cost
32 Profit
33 Sales

With the help of factory overhead , administration overhead & selling and distribution overhead we
can characterise the cost sheet and the total sales of laxmi soap factory is -----------.
With the help of this information we can easily identify :-
 Pvr
 Breakeven point in rupees
 Breakeven point in units

Quiz:

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1. Soaps are _____________ based soapy detergents.

a) Water
b) Kerosene
c) Oil
d) Acid

2. The saponification of a fat or oil is done using _______________ solution for hot
process.
a) KOH
b) NaOH
c) HCl
d) NaCl

3. The saponification of a fat or oil is done using _______________ solution for cold
process.
a) KOH
b) NaOH
c) HCl
d) NaCl

4. Soft soaps are the limitation of hot process because of their ____________
a) High alkalinity
b) Low alkalinity
c) Low solubility in water
d) High solubility in water

5. Select the incorrect statement from the following option.

a) Hard soaps are the sodium carboxylates
b) Soft soaps are potassium carboxylates
c) Hard soaps are manufactured by cold process
d) Example of soft soap – shampoo and shaving cream

6. Which of the following is the residual product in the formation of soap?

a) Glyceraldehyde
b) Glycerol
c) Glycerine
d) Acrylonitrile

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7. Which of the following is a typical soap molecule?

a) Calcium stearate
b) Potassium permanganate
c) Sodium bicarbonate
d) Sodium stearate

8. Select the correct statement from the following options.

a) The soap micelle is unstable due to positive charge on its head
b) The soap micelle is stable due to positive charge on its head
c) The soap micelle is unstable due to negative charge on its head
d) The soap micelle is stable due to negative charge on its head

9. Soaps do not act efficiently in hard water and in acidic solution.

a) True
b) False

Marks: Signature:

Experiment No.: …2….. Date: ………..

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Preparation of detergent

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

Materials Required:
Dodecanol (dodecyl alcohol) C12H25OH, Sulfuric acid, concentrated Sodium hydroxide 6M,
Phenolphthalein solution 1%, Sodium chloride, technical grade Erlenmeyer flask 125-mL,
Beakers 400-mL, 150-mL, 100-mL, Graduated cylinders 10-mL, 25-mL, 125-mL, Funnel,
Spatula, Stirring rod Cheesecloth, Watch glass, Scissors

Theory:
Any substance that is used to clean the laundry is called detergent. There are different types of
detergent used depending upon the type of laundry, the amount of dirt in them, and the
hardness of stains or as per the requirements of the cloth. Most often, when we speak of
laundry, we are generally concerned with what it is, our clothes, sheets, towels or that matter
even our shoes! But ever thought about the product used to wash them all? Well, if not, it high
time that we'll go through a whole bunch of different types of detergent available today.

DIY: DIY homemade laundry detergents are an easy way to save some bucks. You can give
them the fragrance of your choice and select the ingredients as per your comfort and skin
suitability. Though they are organic with no toxins and harsh chemicals and last for long, yet
they come with their own share of difficulties and challenges. The DIY detergents are less
convenient, less effective and efficient than the conventional detergents, take time and are
messy to prepare.

Conventional Detergent: Conventional Laundry detergent, like any other household product,
can contain toxic chemicals and even carcinogens. The conventional detergents use chemicals
to bring fragrance, the cleaning agents to make the laundry cleaner, the stabilizers to stabilize
their shelf life, and bleach, brighteners and phosphates to make the detergents more effective
in hard water. Their remains are found to be there on the clothes even after washing and are
likely to come into contact with skin, causing irritation.

Non Toxic detergent Pods: Non-Toxic detergent pods are free from chemicals and are easy
to use. They free the user from the chaos of using the correct dose, which often happens
naturally. Cleancult is one such non-toxic detergent. It is highly effective and is a box of
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sensitive laundry pods that combine cleaning, stain removal, and brighteners. The best part is
that it is free of Chlorine, Dyes, Phosphates, and Masking Agents. It has also achieved a
cleaning rating equivalent to conventional detergents. Since these are hypoallergenic and great
for sensitive skin, you can sit, relax and know that you can have clean laundry with great and
skin friendly ingredients.

Hand wash powder detergent is designed for washing clothes by hand or with a semi-
automatic washing machine. Like Ariel Complete, it produces more suds than other
detergents, and works to remove stains from your clothes even without the extra agitation
you’d get from a fully-automatic washing machine.

Machine washing powder, designed for fully-automatic washing machines, is great if you’re
looking to see bright whites. Since these powder detergents are better for fully-automatic
washing machines (which use less water than you typically would while hand washing), the
detergent produces less suds. Powder detergents, such as Ariel Matic, come with more active
ingredients than hand wash detergents – for example, bleaching technology. Powder is
especially effective at removing outdoor stains or ground-in dirt.

Liquid detergent is also designed with fully-automatic washing machines in mind and is
convenient for directly treating stains, as you can simply pour it onto the stain and let it pre-
treat before washing. If you’re battling oil and grease, liquid detergent is a great choice. It’s
worth noting that some ingredients used in powder, like non-chlorine bleach (which make
whites bright), aren’t included in the liquid form, so liquid may not be the ideal choice if
you’re looking for bright whites. However, if you’re interested in keeping your colours bright,
liquid is the perfect detergent for removing stains while protecting colours.

Procedure:
1. Place 5 ml of dodecanol into a 100-mL beaker.
2. Measure 2 mL of concentrated sulfuric acid, H2SO4, in a 10-mL graduated cylinder.
3. With stirring, slowly add the 2 mL of concentrated sulfuric acid to the dodecanol in the
beaker. Continue to stir for 1 minute after addition of the sulfuric acid is complete. Let the
mixture stand for 10 minutes.
4. Fill a 250-mL beaker one-third full of ice, add about 10 g of sodium chloride, NaCl, and
mix thoroughly. Add water to bring the total volume of the mixture to 75 ml.
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5. Mix 5 ml of 6 M sodium hydroxide with 10 mL of water in a small beaker. Mix well, then
add 4 drops of phenolphthalein indicator. The pink color of the phenolphthalein may begin
to fade in the strongly basic solution.
6. Prepare a mixture of about 25 mL of ice water.
7. After the 10 minutes, carefully pour the sodium hydroxide solution into the dodecanol-
sulfuric acid mixture. Stir until the pink color disappears. A large amount of solid
detergent should form.
8. Pour the detergent mixture into the ice-salt bath. Stir to break up large lumps of detergent.
9. Filter the precipitated detergent mixture through 2-3 layers of cheesecloth in a funnel
mounted on a ring stand.
10. Wash the collected detergent twice with 10 ml portions of ice-cold water.
11. Remove the cheesecloth from the funnel, squeeze excess water from the solid detergent,
and save the detergent for use in Part C.

Precautions:
1. As it is heating, some of the solution will evaporate. You must make sure that the
volume does not decrease too much, so you will need to add more liquid as the reaction
progresses. Add 5 mL portions of a mixture containing equal volumes of ethanol and
water to the beaker in order to maintain the same volume in the beaker. Also, do not let
the mixture overheat or foam over, and do not allow it to boil to dryness! If this
happens, you will need to start over.
2. Caution: the mixture of oil and ethanol will be very hot, and may splatter or catch fire.
Have a watch glass nearby to smother any flames. Wear goggles at all times, because
NaOH can cause permanent eye damage!
3. The soap may still contain NaOH, so avoid skin contact with it. Use plastic gloves if
possible.) Leave the soap to dry in your locker until the next laboratory period.
4. Ethanol is flammable. Keep the container covered and take care to avoid flames.
5. Sulfuric acid is extremely corrosive and can cause severe burns. In the event of skin
contact, immediately rinse the affected area with water. If any gets on your clothes,
remove the affected item of clothing and wash both the clothing and the area of
suspected skin contact. If skin is blistered or broken, consult qualified medical
assistance.
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Cost Analysis:
Units of production = -----------

Sr. No. Particular Per unit price Total

1 DIRECT MATERIAL
2 Acids
3 Speciality chemicals
4 Ordinary chemicals
5 Perfumes
6 Direct labour
7 Direct expense
8 Pirme Cost
Factory overheads (Fixed)
9 Depreciation
10 Rent
11 Power
12 Insurance
13 Supervisors salary
Factory overheads (variables)
14 Electricity
15 Running exp. Of machine
16 Work cost/ factory cost
Office overheads:
17 Employee cost
18 Computer
19 Telephone
21 Taxes
22 Carriage out ward
23 Cost of production
24 opening stock of finished
goods
25 -Closing stock of finished
goods
26 Cost of goods sold
Selling & distribution overheads:
27 Advertisement
28 Delivery vehicles
29 Petrol
30 Packaging rates
31 Cost of sales / total cost
32 Profit
33 Sales

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With the help of factory overhead , administration overhead & selling and distribution overhead we
can characterise the cost sheet and the total sales of laxmi soap factory is -----------.
With the help of this information we can easily identify :-
 Pvr
 Breakeven point in rupees
 Breakeven point in units

Quiz:
1. Soap was invented as long ago as:
a. 200 years
b. 1000 years
c. 2000 years
2. Soaps were originally made from:
a. Proteins
b. Animal fats and vegetable oils
c. Chemicals extracted from the soil
3. Today's soaps are synthesised from products including:
a. Plastics
b. Sodium hydroxide and alcohol
c. Proteins and hydrochloric acid
4. In a school laboratory, soap is usually made from:
a. Vegetable oil, sodium hydroxide and some alcohol
b. Methylated spirits (also called denatured alcohol) and any acid
c. Acids and caustic soda
5. Soaps work because the "water-loving" end of the soap molecule attracts a water molecule
and the "water-hating" end attracts:
a. Other soap molecules
b. Water molecules also
c. Grease or dirt
6. The scientific term for "water-loving" is:
a. Hydrophilic
b. Hydroxide
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c. Hydrophobic
7. The scientific term for "water-hating" is:
a. Hydroxide
b. Hydrophilic
c. Hydrophobic

8. The "water-loving" end of the soap molecule has a charge that is:
a. Positive
b. Negative
c. Either positive or negative
9. The water-repelling end of the soap molecule has a:
a. Negative charge
b. Positive charge
c. Neutral or no charge

Marks: Signature:

Experiment No.: …3….. Date: ………..

Saponification Value

Objective: To determine saponification value of oil sample

Material Required:
Fats and Oils [coconut  oil, sunflower oil], Conical Flask, 100ml beaker, Weigh Balance,
Dropper, Reflux condenser, Boiling Water bath, Glass pipette (25ml), Burette, Ethanolic

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KOH(95% ethanol, v/v), Potassium hydroxide [0.5N], Fat solvent, Hydrochloric acid[0.5N],
Phenolphthalein indicator.
Theory:
Fats and oils are the principle stored forms of energy in many organisms. They are highly
reduced compounds and are derivatives of fatty acids.  Fatty acids are carboxylic acids with
hydrocarbon chains of 4 to 36 carbons; they can be saturated or unsaturated.  The simplest
lipids constructed from fatty acids are  triacylglycerols or triglycerides.  Triacylglycerols are

composed of three fatty acids each in ester linkage with a single glycerol.  Since the polar
hydroxyls of glycerol and the polar carboxylates of the fatty acids are bound in ester linkages,
triacyl glycerols are non-polar, hydrophobic molecules, which are insoluble in water.

Saponification is the hydrolysis of fats or oils under basic conditions to afford glycerol and the
salt of the corresponding fatty acid.   Saponification literally means "soap making". It  is
important to the industrial user to know the amount of free fatty acid present, since this
determines in large measure the refining loss. The amount of free fatty acid is estimated by
determining the quantity of alkali that must be added to the fat to render it neutral. This is
done by warming a known amount of the fat with strong aqueous caustic soda solution, which
converts the free fatty acid into soap.  This soap is then removed and the amount of fat
remaining is then determined. The loss is estimated by subtracting this amount from the
amount of fat originally taken for the test.
 The saponification number is the number of milligrams of potassium hydroxide  required to
neutralize the fatty acids  resulting from the complete hydrolysis of 1g of fat .    It gives
information concerning the character of the fatty acids of the fat- the longer the carbon chain,
the less acid is liberated per gram of fat hydrolysed. It is also considered  as a  measure of the
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average molecular weight (or chain length) of all the fatty acids present.  The long chain fatty
acids found in fats have low saponification value because they have a relatively fewer number
of carboxylic functional groups per unit mass of the fat and therefore high molecular weight.

Fats (triglycerides) upon alkaline hydrolysis (either with KOH or NaOH ) yield glycerol and
potassium or sodium salts of fatty acids (soap) .  
 

 
Procedure:

1. Weigh 1g of fat in a tarred beaker and dissolve in about 3ml of the fat solvent
[ethanol/ether mixture].
2. Quantitatively transfer the contents of the beaker three times with a further 7ml of the
solvent.
3. Add 25ml of 0.5N alcoholic KOH and mix well, attach this to a reflux condenser.
4. Set up another reflux condenser as the blank with all other reagents present except the
fat.
5. Place both the flasks in a boiling water bath for 30 minutes.
6. Cool the flasks to room temperature.
7. Now add phenolphthalein indicator to both the flasks and titrate with 0.5N HCl.
8. Note down the endpoint of blank and test .
9. The difference between the blank and test reading gives the number of millilitres of
0.5N KOH required to saponify 1g of fat.
Calculations:
         Saponification value or number of fat = mg of KOH consumed  by 1g of fat.

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         Weight of KOH = Normality of KOH * Equivalent weight* volume  of KOH in litres

         Volume of  KOH consumed by 1g  fat = [-----------------]ml

Quiz:
1. Saponification is the value of oil for which the number of mgs of KOH required to
saponify the ________ present in the 1g of oil.
a) Fatty materials
b) Salts
c) Free acids
d) Bases
2. 2. It is __________ of fatty oils which leads to formation of soaps.
a) Alkaline hydrolysis
b) Alkaline electrolysis
c) Hydrolysis
d) Electrolysis
3. 3. Which of the following is not saponifiable?
a) Ground nut oils
b) Mineral oils
c) Castor oil
d) Coconut oil
4. 4. ________ get large amount of alkali to hydrolysis.
a) Baby oil
b) Liquid paraffin
c) Vegetable oil
d) Liquid petroleum
5. 5. The saponification value of the vegetable oil is _______
a) Very high
b) Very low
c) Moderate
d) Cannot be determined
6. 6. The different properties of the soaps is due to the ___________
a) Nature of alkali
b) Nature of the oil
c) Temperature variance
d) Nature of the fats
7. 7. Hard soaps can be formed by using ______
a) KCl
b) NaCl
c) KOH
d) NaOH
8. 8. The deformations caused in oil paintings are due to saponification.
a) True
b) False
9. 9. Fatty acids have _____ inter molecular forces.
a) Weak
b) Strong
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c) No
d) Very strong
10. 10. The mixtures derived from the diverse fatty acids are _________
a) Glycerides
b) Bi glycerides
c) Triglycerides
d) Polyglycerides

Marks: Signature:

Experiment No.: …4….. Date: ………..

Acid Value of Oil

Objective: To determine the acid value of the given sample of oil.

Materials Required:
250 mL conical flasks, Phenolphthalein indicator solution, Alkali Blue 6B indicator solution,
Ethyl alcohol, sodium hydroxide solution.
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Theory:
The acid value is defined as the number of milligrams of Potassium hydroxide required to
neutralize the free fatty acids present in one gram of fat. It is a relative measure of rancidity
as free fatty acids are normally formed during decomposition of triglycerides. The value is
also expressed as per cent of free fatty acids calculated as oleic acid, lauric, ricinoleic and
palmitic acids.
The acid value is determined by directly titrating the oil/fat in an alcoholic medium against
standard potassium hydroxide/sodium hydroxide solution.
The value is a measure of the amount of fatty acids, which have been liberated by hydrolysis
from the glycerides due to the action of moisture, temperature and/or lipolytic enzyme lipase.

Procedure:
Mix the oil or melted fat thoroughly before weighing. The mass of the test sample
shall be taken based on the colour and expected acid value.
Expected Acid Mass of Test portion Accuracy of weighing of
Value test portion (gm)
(gm)
<1 20 0.05

1 to 4 10 0.02

4 to 15 2.5 0.01

15 to 75 0.5 0.001

>75 0.1 0.0002

a) Weigh accurately appropriate amount of the cooled oil sample as mentioned in the above
table in a 250 mL conical flask.
b) Add 50 mL of freshly neutralized hot ethyl alcohol and about one ml of phenolphthalein
indicator solution. In case of rice bran oil or RBO based blends, add about 1mL of Alkali
blue indicator.
c) Heat the mixture for about fifteen minutes in water bath (75-80°C)
In case of Rice bran oil or RBO based blended oils or fats, add 1mL of Alkali blue
indicator after heating.
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d) Titrate while hot against standard alkali solution shaking vigorously during the titration.
e) End point using phenolphthalein indicator shall be from colourless to light pink
(Persisting for 15 sec.)
f) End point using Alkali blue 6B indicator shall be disappearance of blue colour which
developed during addition of indicator.
Note: Noting burette reading after “obtaining dark pink colour OR Orangish red” as end
point should be avoided as it will lead to erroneous result
g) The weight of the oil/fat taken for the estimation and the strength of the alkali used for
titration shall be such that the volume of alkali required for the titration does not exceed
10mL.

Calculation:
56.1Vx N
Acid value =
W
Where,

V = Volume in mL of standard potassium hydroxide or sodium hydroxide used

N = Normality of the potassium hydroxide solution or Sodium hydroxide solution; and
W = Weight in gm of the sample

Quiz:
1. Suppose that 40.00 cm3 of 0.020 M KOH is titrated with 0.030 M HNO3. Find the pH of the
solution in the flask (a) before any HNO3 is added; (b) halfway to the endpoint; (c) one drop
(0.05 cm3) before the endpoint; (d) one drop after the endpoint.
Solution
a) Since KOH is a strong base, [OH–] = 0.020 = 2 x 10–2. Thus

 and 
b) Halfway to the endpoint means that half the OH– has been consumed. The original amount of
OH– was so the amount remaining is 0.4 mmol OH–. It must have required 0.4 mmol HNO3 to
consume the other 0.4 mmol OH–, and so the volume of HNO3 added is
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 The total volume of solution at this point is thus (13.33 + 40.00) cm3 = 53.33 cm3, and
 and
 c) If the total volume of of HNO3 required to react with all the OH- in solution is 26.66 cm3,
when 26.61 cm3 of HNO3 solution have been added, the amount of H3O+ added is
 This would consume an equal amount of OH–, and so the amount of OH– remaining is (0.8 –
0.798) mmol = 0.002 mmol. Thus
 and 
 d) An excess of 0.05 cm3 of acid will add of H3O+ to a neutral solution whose volume is (40.00
+ 26.71)cm3 = 66.71 cm3.
2. Ten grams of olive oil are dispersed in 50 cm 3 ethanol for a final volume of 60.86 cm 3. The
mixture is titrated with 50 cm3 KOH 0.1 M. a) What is the AV of this sample of olive oil?
Assuming that the only free fatty acid present in the sample is oleic acid and that we are working
with an aqueous solution at all times, what is the pH of the mixture b) before any KOH is
added?, when c) 10 cm3, d) 25 cm3, e) 35 cm3 e) an excess of 1.5cm3 KOH 0.1 M have been
added?
Note: Oleic acid (c-9-octadecenoic) pKa=9.85[5]

Solution
a) If 50 cm3 of 0.1 M KOH were used to neutralize the sample, the number of moles of KOH is
 The molar mass of KOH is 56.10 g/mol and the mass of KOH employed in mg is this amount of
KOH was used to neutralize 10 g of olive oil. The acid value is the then This AV is considerable
higher than the one shown in the table above. What does this tell you about the oil?
This oil has probably been heated (cooking/frying), it is old, or it has been stored under
conditions favoring lipase activity. In the case of refined oils, a high AV indicates inappropriate
or incomplete refining procedures.
b) From the number of moles of KOH employed to neutralize the oil we can conclude that there
were 5.0 mmol of oleic acid in the sample and the ethanolic dispersion. Given that the volume of
the dispersion was 60.83 cm3 the concentration of oleic acid is then
 Using equation (5) from Weak acids in foods - pH and beyond
c) When 10 cm3 of KOH solution had been added, the volume of the dispersion is 60.83 + 10 =
70.83 cm3 and the corresponding number of moles of OH - is  This means that 1.0 mmol of oleic

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acid have reacted and produced 1.0 mmol of oleate, its conjugate base. At this point, the number
of moles of oleic acid and oleate are  and their concentrations  Since we have both the acid and
its conjugate base in the dispersion we can use the Henderson-Hasselbach equation to calculate
the pH 
 Note that all the OH- has reacted with oleic acid and it is not present in the dispersion.
 d) When 25 cm3 have been added, we are halfway to the equivalence point. Half of the oleic
acid has been converted into oleate and their concentrations are equal.   Again, we have both the
acid and its conjugate base in dispersion and we use the Henderson-Hasselbach equation  So
halfway the equivalence point 
 e) If 35 cm3 0.1 KOH have been added  So 3.5 mmol of oleic acid have been converted into
oleate and 1.5 remain in the dispersion. With a new volume of 95.83 cm 3, their corresponding
concentrations are and  
f) If an excess of 1.5 cm3 are added to the dispersion, its final volume is 112.33 cm3. Since all the
oleic acid has been converted into oleate, there are no more protons to react with the OH - ions
and it will remain in solution.
The number of moles of OH- ions is for a concentration of Since the OH- is the strongest base in
solution, it will govern the pH of the reaction mixture. The concentration of OH- generated by
oleate is negligible, so we calculate the pH of the dispersion as
and
 Notice the assumptions we made to calculate pH at different stages of this titration. Initially, the
oil is dispersed in ethanol, the dissociation constants of acids change depending on the medium
and strictly speaking it is probably incorrect to talk about pH in this conditions. The method is
also based on the assumption that protons are in the interface ethanol-water and readily react
with aqueous NaOH. These are some of the limitations of the method and the reason for the need
of a titration instead of direct measurement of pH on the sample.

1. Which product is produced when ghee is heated with crystals of potassium bisulphate?
a. Benzaldehyde
b. Ethanol
c. Formaldehyde
d. Acrolein

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2. Rose red colour appears when vanaspati ghee is subjected to Baudouin test. What does it
indicate?
a. Presence of olive oil
b. Presence of sunflower oil
c. Presence of seasame oil
d. Presence of mustard oil
3. Which one of the following tests is used to determine the degree of unsaturation in the
given sample of oil or fat?
a. Baudouin test
b. Iodine test
c. Acrolein test
d. Huble’s test
4. What is the process of slow oxidation of fats and oils present in the food materials
resulting in some bad smelling compounds called?
a. Hydrolysis
b. Hydrogenation
c. Rancidity
d. Carboxylation
5. What are the decomposition products of fats?
a. Glycerol and hydrochloric acid
b. Glycerol and sulphuric acid
c. Glycerol and higher fatty acids
d. Glycerol and acetic acid
6. Which one of the following tests is used to determine the presence of seasame oil in a
given sample of ghee?
a. Translucent spot test
b. Huble's test
c. Baudouin test
d. Acrolein test
7. Which one of the following reagents is used to test the presence of unsaturation in the
given sample of oil or fat?
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a. Alcohol
b. Potassium bisulphate solution
c. Huble's reagent
d. Furfuraldehyde
8. What is acrolein?
a. An unsaturated aldehyde
b. A ketone
c. An alcohol
d. A hydrocarbon

Marks: Signature:

Experiment No.: …5….. Date: ………..

Preparation of Calcium Carbonate

Objective: To prepare hydrated lime from the given calcium carbonate powder
Materials Required:
Ethanol, Glycerin, Di water, Baker, Ostwald viscometer, Pipet

Theory:
Calcium carbonate is one of the most popular chemicals which is first encountered in school
classrooms, where the use of chalk (a form of CaCO3) is found. It is found in the earth’s
crust.  It is also found in many forms such as marble, limestone, etc. Although they are
available in various forms they are chemically similar and only differ physically. They are
also referred to as calcite.

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Calcium carbonate is a non-toxic and odourless compound commonly found as a white

mineral which occurs naturally in chalks, limestones and marbles.
Calcium carbonate is produced commercially in two different grades. Both grades compete
industrially based primarily on particle size and the characteristics imparted to a product.
1. Ground Calcium Carbonate – Produced via extraction and processing of naturally
occurring deposits. GCC crystal shape is irregularly rhombohedral and has a broader size
distribution.
2. Precipitated Calcium Carbonate – Produced via chemical precipitation via a carbocation
process or as a by-product of some bulk chemical processes. PCC crystal shape depends
on the product and the product and the particles are more uniform and regular with a
narrow size distribution.
PCC has smaller particles has a higher purity is less abrasive and tends to have higher
brightness than GCC.

Procedure:
1. CaCO3 is obtained by using carbon dioxide and slaked lime as raw materials. When
carbon dioxide is passed through slaked lime, calcite is obtained.
Another method to obtain calcite is by adding sodium carbonate to calcium chloride.
                  Ca (OH)2 + CO2 → CaCO3 + H2O
                 CaCl2 + Na2CO3 → CaCO3 + 2NaCl
When carbon dioxide is passed in excess it leads to the formation of calcium hydrogen-
carbonate.

2. On a large scale, it is prepared by passing carbon dioxide gas through calcium

hydroxide (slaked lime). However, if carbon dioxide is passed in excess, it forms the
soluble calcium hydrogen-carbonate.

Ca(OH)2 + CO2→ CaCO3 + H2O

Properties of CaCO3
 It is a fluffy powder.
 It decomposes to give carbon dioxide when heated up to 1200K.

 When it reacts with dilute acid, it liberates carbon dioxide as a by-product.

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                 CaCO3+H2SO4 → CaSO4+H2O+CO2
 At 1200K, calcium carbonate decomposes to give carbon dioxide and calcium oxide.
CaCO3 → CaO + CO2

 On reacting with dilute acids, calcium carbonate gives carbon dioxide.

CaCO3 + 2HCl → CaCl2 + H2O +CO2

Application of Calcium Carbonate

 Calcium carbonate is largely employed in the pulp and paper industry. It can be used as a
filter and pigment, making possible the production of a whiter, higher quality pigment
than other minerals.

 In the construction industry, calcium carbonate is used as a filler in concrete, increasing

its durability and appearance and to purify metals for use in construction applications.

 Another application of calcium carbonate is in fertilizers to provide calcium to plants and

pH stabilization of the soil.

 Calcium carbonate can also be an additive to food products for livestock animals and
humans and as a supplement in vitamins.

 In water and sewer treatment plants, calcium carbonate is employed in the removal of
acidity and impurities.

Calcium Carbonate Uses

The list of uses of calcium carbonate is given below.
 It plays an important role in construction, be it as a building material (marble) or as an
ingredient in cement.
 It is used in medicinal industries which manufacture antacids, tablets which are made of
base materials etc.

 It is used as calcium supplements.

 It is used in the manufacture of paints, paper, plastics, etc.

Quiz:

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1. What is the calcium carbonate used for?

Ans: It used as an antacid is calcium carbonate to alleviate heartburn, acid indigestion, and
stomach upset.
2. Name the fruit which is rich in calcium?
Ans: Apricot, gooseberry, figs, raisins are the fruits rich in calcium.
3. Is Limestone a calcium carbonate?
Ans: It is a sedimentary carbonate rock that often consists of skeletal parts of marine
organisms such as coral, foraminiferous, and molluscs.
4. How do you identify carbonate salt?
Ans: Strong acids, such as hydrochloric acid, can be added to assess whether a mineral or
rock contains calcium carbonate. If the sample contains calcium carbonate, carbon dioxide
will be fizzed and produced.
5. What is the formula for calcium carbonate?
Ans: The formula for calcium carbonate is CaCO3.

Marks: Signature:

Experiment No.: …6….. Date: ………..

Synthesis of Aspirin
Objective: To synthesis aspirin from salicylic acid.
Materials Required:
Goggles 250 mL ice bath Salicylic Acid 50 mL Erlenmeyer Flask
Gloves 250 mL hot water bath Acetic Anhydride Vacuum filter apparatus
Lab coat Stirring rod 2 Watch glasses 2 pieces of round filter paper
Distilled Water 110-mm Filter paper 10 mL Ethanol, 85% Phosphoric Acid
TLC plate Spotting pipettes Silica gel coated 2 mL methylene chloride
Ruler 400 mL beaker 18 mL Ethyl acetate 125 mL Erlenmeyer Flask
UV light

Theory:

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Over history, many compounds obtained from nature have been used to cure ills or to produce
an effect in humans. These natural products have been obtained from plants, minerals, and
animals. In addition, various transformations of these and other compounds have led to even
more medically useful compounds. During this semester, you will have an opportunity to
isolate some pharmacologically active natural products and to synthesize other active
compounds from suitable starting materials. Analgesics are compounds used to reduce pain,
antipyretics are compounds used to reduce fever. One popular drug that does both is aspirin.
The Merck Index, which is an encyclopedia of chemicals, drugs and biologicals, lists the
following information under aspirin: acetylsalicylic acid; monoclinic tablets or needle-like
crystals; mp 135 °C (rapid heating); is odorless, but in moist air it is gradually hydrolyzed into
salicylic and acetic acids; one gram dissolves in 300 mL of water at 25 °C, in 100 mL of water
at 37 °C, in 5 mL alcohol, in 17 mL chloroform.

Mechanism of the reaction (Acetylation of Salicylic Acid)

One method for the preparation of acetylsalicylic acid involves the acylation of salicylic
acid as shown in figure 2. The acylating agent is acetic anhydride, which in the presence
of an acid catalyst reacts with salicylic acid to provide acetylsalicylic acid in an
excellent yield. First, acetic anhydride is protonated by the acid to form an activated
carbonyl species. Next, a lone pair from the salicylic acid OH attacks the carbonyl
carbon of the activated electrophile. A proton is then transferred from the aromatic
oxygen to the ester oxygen. Next, acetic acid (CH 3COOH) is dispelled. The resulting
protonated ester loses its proton upon reaction with a weak base to provide
acetylsalicylic acid.

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Mechanism for the Acylation of Salicylic Acid

Procedure:
1. Place 2.0 g (0.015 mole) of salicylic acid in a 125-mL Erlenmeyer flask.
2. Add 5 mL (0.05 mole) of acetic anhydride, followed by 5 drops of conc. H2SO4 (use a
dropper, H2SO4 is highly corrosive) and swirl the flask gently until the salicylic acid
dissolves.
3. Heat the flask gently on the steam bath for at least 10 minutes.
4. Allow the flask to cool to room temperature. If acetylsalicylic acid does not begin to
crystallize out, scratch the walls of the flask with a glass rod. Cool the mixture slightly in
an ice bath until crystallization is completed. The product will appear as a solid mass when
crystallization is completed.
5. Add 50 mL of water and cool the mixture in an ice bath. Do not add the water until
crystal formation is complete.
6. Vacuum filter the product using a Buchner funnel. You can use some of the filtrate to
rinse the Erlenmeyer flask if necessary.
7. Rinse the crystals several times with small portions (5 mL) of cold water and air dry the
crystals on a Buchner funnel by suction until the crystals appear to be free of solvent. Test

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this crude product for the presence of unreacted salicylic acid using the ferric chloride test.
Record the weight of the crude solid which probably contains water.
8. Stir the crude solid with 25 mL of a saturated aqueous sodium bicarbonate solution in a
150 mL beaker until all signs of reaction have ceased (evolution of CO2CO2 ceases).
9. Filter the solution through a Buchner funnel to remove any insoluble impurities or
polymers that may have been formed. Wash the beaker and the funnel with 5 to 10 mL of
water.
10. Carefully pour the filtrate with stirring, a small amount at a time, into an ice cold HCl
solution (ca 3.5 mL of conc. HCl in 10 mL of water) in a 150-mL beaker and cool the
mixture in an ice bath. Make sure that the resulting solution is acidic (blue litmus paper)
and that the aspirin has completely precipitated out.
11. Filter the solid by suction and wash the crystals 3X with 5 mL of cold water each.
Remove all the liquid from the crystals by pressing with a clean stopper or cork. Air dry
the crystals and transfer them to a watch glass to dry. Test a small amount of the product
for the presence of unreacted salicylic acid using the ferric chloride solution.
12. When the product is completely dry, weigh the product, determine its melting point (lit
mp 135-136 °C) and calculate the percentage yield.
13. Dissolve the final product in a minimum amount (no more than 2-3 mL) of hot ethyl
acetate in a 25 mL Erlenmeyer flask. Make sure that the product is completely dissolved
while gently and continuously heating on a steam bath.
14. Cool the solution to room temperature and then in a ice-bath. Collect the product by
vacuum filtration and rinse out of the flask with a few milliliters of cold petroleum ether.
15. When the product is completely dry, weigh its weight, determine its melting point (lit mp
135 °C) and calculate the percentage yield of this recrystallized product. Calculate the %
recovery of recrystallized material from crude material. Submit the crystalline sample in a
small vial with proper labeling to your instructor

Ferric Chloride Test For Salicylic Acid: Add 10 drops of aqueous 1% ferric chloride solution to
a test tube containing a few crystals of the compound to be tested dissolved in 5 mL water and note the
color. Do this test with 1.phenol, 2. salicylic acid, and 3. your crude product. Formation of an iron-

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phenol complex with Fe(lll) gives a definite color ranging from red to violet, depending upon the
particular phenol present.
IR-spectrum: In aspirin 1 we expect: sec. alcohols, anhydrides and carboxylic acids. In
aspirin 2 we expect: esters, alkyl groups and aromatic ethers. It does not quite match, but we
can confirm the fact that aspirin has formed. The peak at 1256 is an indicator for a aromatic
ether. And the peak at 1749 is an indicator for an ester. Those were both not present in the
salicylic acid. The secondary alcohol from salicylic acid could be an other difference.
However my aspirin 1 was failed.
H-NMR: Via the H NMR spectrum you can see that aspirin was formed. On the print I
explained which peak stands for which H-atom. You can see 6 regions, but there are 7 regions
(A-F). The steep high single peak at 2,351 is the CH3(A) group, because there are the 3 H+
atoms in the same signal. The double, triple, triple, double peaks are from the benzene

Quiz:
1. Use the structural formulas to write the chemical equation to show how
acetylsalicylic acid is synthesized from salicylic acid and acetic anhydride.

2. Calculate the molar mass of salicylic acid and acetylsalicylic acid.

3. Calculate the theoretical yield of acetylsalicylic acid from 2.01 g of salicylic acid
assuming excess acetic anhydride.

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4. Assume that 1.93 g of acetylsalicylic acid is produced from the reaction in the
previous question. Calculate the percent yield.

Marks: Signature

Experiment No.: …7….. Date: ………..

Preparation of phenyl azo – β – Naphthol
Objective: Preparation of phenyl azo – β – Naphthol from aniline
Material Required:
1. Aniline 2. Sodium nitrite 3. Hydrochloric
acid
4. 2-Naphthol 5. Sodium hydroxide 6. Beaker
solution
7. Test tube 8. Buchner funnel 9. Pipette
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10. Capillary tube 11. Thermometer 12. Distilled

water
13. Hot air oven 14. Ice bath

Theory:
2- Naphthol aniline dye is a scarlet dye can be prepared by coupling reaction. Aniline reacts
with sodium nitrite in the presence of hydrochloric acid forms benzene diazonium chloride.
Further benzene diazonium chloride reacts with 2-naphthol forms a bright orange colour 2-
naphthol aniline dye.
Azo compounds are prepared by the reaction of diazonium salts with phenol under alkaline
conditions. Primary aromatic amines react with nitrous acid at 0oC to give a diazonium salt.

Nitrous acid is in turn formed by the reaction of sodium nitrite with hydrochloric acid. The
active reagent is nitrous anhydride or dinitrogen trioxide. Nitrous anhydride reacts with
aniline to give nitroamine derivative which is unstable and isomerizes to form a diacetic acid
which in turn converted to a diazonium salt. Finally, this diazonium salt reacts with 2-
naphthol in the presence of sodium hydroxide give 2-naphthol aniline which is an aniline dye.

Procedure:
1. Dissolve 5ml of aniline in a mixture of concentrated hydrochloric acid and water.
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2. Cool the solution in ice bath between 0-5oC.

3. Add a solution of 4gm sodium nitrite in 15ml of water drop-wise with continuous shaking
and controlling the temperature below 5oC.
4. Take another flask to dissolve 8gm of 2-naphthol in a solution of 5 gm sodium
hydroxide solution in 50ml of water.
5. Cool the solution in the ice bath to 0-5oC.
6. Now mix the two cold solutions slowly drop wise with constant stirring.
7. Continue the stirring at least half an hour without allowing the temperature to rise above
10oC.
8. An orange colour azo dye called 2-naphthol aniline separates out.
9. Filter the crude sample and wash it with cold water.
10. Dry and recrystallize it from ethyl alcohol or glacial acetic acid.

Calculation of the Practical yield:

93 g of aniline reacting with 144 g of β – Naphthol yields the phenylazo β Naphthol =
258g
10 g of aniline shall yield phenyl azo – β – Naphthol = (258/93) x 10 = 27.74g
Therefore, theoretical yield of phenyl azo – β – Naphthol is 27.74g
If reported practical yield = 9.5g
Then, the percentage practical yield = (practical yield/ theoretical yield)x100
= (9.5/27.74)x100 =34.25%
Precautions:
1. The solution of the aniline hydrochloride should be cooled to 5˚C, and this
temperature should be maintained throughout the addition of sodium nitrate solution.
2. Addition of sodium nitrate should be very slow because the reaction is highly
exothermic and may cause the temperature to rise.
3. Always add the diazonium chloride solution to β – Naphthol solution for dye
formation and not vice versa.

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4. The solution of the aniline

hydrochloride should be
cooled to 5°C, and this
5. temperature should be
maintained throughout the
addition of the sodium
6. nitrite solution.
7. 2. Addition of sodium
nitrite should be very slow
because the reaction is
8. exothermic and may cause
the temperature to rise.
9. 3. Always add
diazonium chloride

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solution to β-naphthol
solution for dye
10. formation and not vice-
versa.
11. 4. Wear a lab coat
12. 5. Wear face mask as
there might be toxic or
irritating fumes around
13. 6. Wear gloves
chemicals might be
corrosive as they cause harm
to our skin.
14. The solution of the
aniline hydrochloride should
be cooled to 5°C, and this
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15. temperature should be

maintained throughout the
addition of the sodium
16. nitrite solution.
17. 2. Addition of sodium
nitrite should be very slow
because the reaction is
18. exothermic and may
cause the temperature to
rise.
19. 3. Always add
diazonium chloride
solution to β-naphthol
solution for dye

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20. formation and not vice-

versa.
21. 4. Wear a lab coat
22. 5. Wear face mask as
there might be toxic or
irritating fumes around
23. 6. Wear gloves
chemicals might be
corrosive as they cause harm
to our skin.
24. The solution of the
aniline hydrochloride should
be cooled to 5°C, and this

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25. temperature should be

maintained throughout the
addition of the sodium
26. nitrite solution.
27. 2. Addition of sodium
nitrite should be very slow
because the reaction is
28. exothermic and may
cause the temperature to
rise.
29. 3. Always add
diazonium chloride
solution to β-naphthol
solution for dye

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30. formation and not vice-

versa.
31. 4. Wear a lab coat
32. 5. Wear face mask as
there might be toxic or
irritating fumes around
33. 6. Wear gloves
chemicals might be
corrosive as they cause harm
to our skin.
34. The solution of the
aniline hydrochloride should
be cooled to 5°C, and this

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35. temperature should be

maintained throughout the
addition of the sodium
36. nitrite solution.
37. 2. Addition of sodium
nitrite should be very slow
because the reaction is
38. exothermic and may
cause the temperature to
rise.
39. 3. Always add
diazonium chloride
solution to β-naphthol
solution for dye

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40. formation and not vice-

versa.
41. 4. Wear a lab coat
42. 5. Wear face mask as
there might be toxic or
irritating fumes around
43. 6. Wear gloves
chemicals might be
corrosive as they cause harm
to our skin.
4. Wear a lab coat.
5. Wear face mask as there might be toxic or irritating fumes around.
6. Wear gloves chemicals might be corrosive as they cause harm to our skin.
Observations and Result:
Colour of the crystals Orange crystals
Expected Yield ------- gm
Melting Point 129-131oC
Quiz:
1. Naphthol differs from naphthalene by the presence of what functional group?
a. Amino group
b. Hydroxyl group
c. Carboxylic acid group
d. Nitro group
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2. 1-Naphthol and 2-naphthol are related to each other in what way?

a. They are cousins of each other
b. They are isomers of each other
c. They are room-mates of each other
d. They are not related at all
3. Naphthol is soluble in alcohol-based solvents primarily because it can:
a. Effectively melt with the solvents.
b. Form London-dispersion forces with the solvent.
c. Hydrogen-bond with the solvent molecules.
d. None of the answer choices are correct.
4. Carbonates' react with dilute acids to produce
a. oxygen
b. carbon dioxide
c. hydrogen
d. water
5. A tincture of iodine is made by dissolving iodine in alcohol which is
a. antiseptic
b. anti inflammatory
c. anti viral
d. anti fungal
6. Neutral substances have pH
a. 3
b. 1
c. 0
d. 7
7. Any solution in which solvent is water, is called
a. aqueous solution
b. hydrated solution
c. anhydrous
d. water solution
8. Bacteria in our mouth are acidic which should be neutralized by
a. toothpaste
b. orange juice
c. vinegar
d. antacid
9. Strong 'alkalis' are
a. highly corrosive

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b. medium corrosive
c. normal corrosive
d. less corrosive
10. Copper sulphate has solubility at 25 ?C in 100 g of water equal to
a. 22g
b. 20g
c. 12g
d. 44g
11.  If an alkali is added to acid, it's acidic nature will be
a. enhanced
b. reduced
c. same
d. constant

Marks: Signature:

Experiment No.: …8….. Date: ………..

Preparaton of mordant dye
Objective: To prepare mordant yellow dye.
Materials Required:
m-Nitroaniline, Salicylic acid, Conc. hydrochloric acid, Sodium-nitrite. beakers, 400 mL
beaker, 20 mL or 50 mL Erlenmeyer flask, 125 mL, with stopper 3 stirring rods graduated
cylinders, 10 mL and 100 mL tongs or forceps beaker tongs metal spatula malachite green p-
nitroaniline tannic acid sodium nitrite, NaNO 2 2-naphthol indigo powder TIS Identification
stain No. 1 TIS Identification stain No. 3A iron(II) sulfate, FeSO 4 sodium hydrosulfite,
Na2S2O4 . 2H2O

Theory:

Dyes are organic compounds that can be used to impart bright, permanent colors to fabrics.
The affinity of a dye for a fabric depends on the chemical structure of the dye and fabric
molecules and on the interactions between them. Chemical bonding thus plays an important
role in how and why dyes work. The chemical structures of six common fabrics—wool,
acrylic, polyester, nylon, cotton, and acetate—are shown in Figure 1 on page 2. Cotton and
wool are natural fibers obtained from plants and animals, while acrylic, polyester, and nylon
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are synthetic fibers made from petrochemicals. Acetate, also called cellulose acetate, is
prepared by chemical modification of natural cellulose. All fabrics, both natural and synthetic,
are polymers.

Polymers are high molecular weight, long chain molecules made up of multiple repeating
units of small molecules. The structures of the repeating units are enclosed in brackets in
Figure 1. The number of repeating units (n) varies depending on the fiber and how it is
prepared. Wool is a protein—a naturally occurring polymer made up of amino acid repeating
units. Many of the amino acid units have acidic or basic side chains that are ionized (charged).
The presence of many charged groups in the structure of wool provides excellent binding sites
for dye molecules, most of which are also charged. Cotton is a polysaccharide composed of
glucose units attached to one other in a very rigid structure.

The presence of three polar hydroxyl (–OH) groups per glucose repeating unit provides
multiple sites for hydrogen bonding to ionic and polar groups in dye molecules. Acetate is
cellulose in which some of the –OH groups have been replaced by acetate groups (–
OCOCH3). The presence of acetate side chains makes acetate softer and easier to work with
than cotton but also provides fewer binding sites for dye molecules. Nylon was the first
completely synthetic fiber. It is a polyamide, made up of hydrocarbon repeating units joined
together by highly polar amide (–CONH–) functional groups. The amide groups provide sites
for hydrogen bonding to dye molecules. The repeating units in polyester are joined together
by ester (–COO–) functional groups. Finally, acrylic fiber is poly(acrylonitrile). Each
repeating unit contains one nitrile (–C———N) functional group.

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Procedure:
A mixture of 7gm of m-nitroaniline, 20ml of conc HCl and 40ml water is prepared in a 500ml
beaker. This is heated until solution is completely clear. Solution is cooled to room
temperature and then to 5˚C with adding 40gm ice prepares a solution of 3.5gm NaNO 2 in
10ml water in a 100ml beaker. Add sodium nitrite solution into above prepared solution
slowly keeping temperature below 5˚C, prepare a solution of 7gm, salicylic acid in 30 ml 20%
Na2CO3. Cool to 5˚C pour diazo solution in salicylic acid at 5˚C. Make the bath alkaline by
adding 20% Na2CO3 solution stir the reaction mixture at 5˚C for 2 hours. Then add 10% NaCl
solution at 45-50˚C till salt dissolved completely, cool and stir at room temperature for one
hour, till complete precipitation of dye. Filter and dry.

Result:
% yield = (Practical yield/ Theoretical yield) 100

1. Theoretical yield: ----------gm.

2. Practical yield: ----------gm.
3. Percentage yield: ----------%

Precautions:
1. Wear safety goggles at all times in the laboratory
2. Wear rubber or plastic gloved to protect your hands from the dyes.
3. The dyes used in this experiment should be handled with the utmost care since they
will dye the skin and clothing. Be careful to keep the dye powders and solutions off
the desk tops. Clean up any spills immediately.
4. Most dye materials are irritants to the skin, eyes, and respiratory system and may be
toxic by inhalation and ingestion. In the event of skin contact, wash the affected area
well with water.
5. Hydrochloric acid is corrosive and can cause severe burns to the skin along with
irritating fumes. Work with the concentrated solution under a hood. In the event of
skin contact, wash the affected area well with water. If the skin is broken or blistered,
seek medical assistance. If irritated by the vapors, get fresh air immediately.
6. Sodium hydroxide is caustic and can cause severe burns to the skin. Do not handle
sodium hydroxide pellets with your hands. In the event of skin contact, wash the
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affected area well with water until there is no soapy feel. If the skin is broken or
blistered, seek medical assistance.
7. Sodium nitrite is an irritant to the skin, eyes, and respiratory system. It is toxic by
ingestion. In the event of skin contact, wash the affected area well with water. Sodium
nitrite can also be an explosion hazard. Do not heat this compound dry or in contact
with any flammable material.
8. Ammonia vapors are irritants to the eyes and respiratory system. Work with the
concentrated solution under a hood. In the event of skin contact, wash the affected area
well with water. If irritated by the vapors, get fresh air immediately.

Quiz:
1. Dyes of 'litmus' are made from
a. rhizoids
b. lichens
c. mycorrhizae
d. algae
2. Antacids that are used for treating indigestion contain
a. potassium hydroxide
b. sodium hydroxide
c. magnesium carbonate
d. magnesium hydroxide
3. Plants absorb mineral salt and fertilizers which are dissolved in
a. air
b. soil
c. water
d. leaves
4. An important factor on which solubility depends, is nature of
a. solvent
b. surface area
c. conditions
d. apparatus
5. If more than one drug is used to treat specific illness, they can be mixed in
a. common solvent
b. different solvents
c. oral dose
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d. one of above
6. If carbon dioxide is passed through limewater it will form
a. white precipitate
b. white smoke
c. acid rain
d. blue flame
7. 'Lactic acid' is present in
a. yogurt
b. lemon
c. apple
d. guava
8. 'Aqueous' solution includes
a. salt solution
b. sugar solution
c. mineral water
d. all of them
9. More accurate and quick measure of "pH" value is given by
a. indicator
b. pH scale
c. pH meter
d. universal indicator
10. Solubility of gases increases with decrease of
a. mass
b. volume
c. temperature
d. pressure

Marks: Signature:

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Experiment No.: …9….. Date: ………..

Disperse dye

Objective: Preparation of disperse dye.

Materials Required:

p-Nitroaniline, Sodium nitrite, sodium carbonate, N,N-Dimethyl aniline conc HCl etc.

Theory:
Disperse dyes are water insoluble non-ionic dyes used to dye man made fibres from acidic
bath, specially designed for dyeing of polyester and are applied alongwith dispersing agent to
retain dyes in fine dispersion
Reaction:

Procedure:

A mixture of 3.5gm p-Nitroaniline, 8ml of water and 10ml of conc. HCl acid is heated until
solution is completely clear. Cool it to room temperature. Then add ice to bring the

temperature at 5oC. Add solution of 1.75gm sodium nitrite in 20ml water slowly. Keep the
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solution in ice bath at 0-5oC. Then pour diazo solution at 0-5 oC in N-N- Dimethylaniline
solution in 25 ml water and 5 ml conc. HCl acid. Add 10% 100 ml NaCl solution. Heat the

mixture to 40-50oC for 15 minutes. Filter and dry.

Result:
% yield = (Practical yield/ Theoretical yield) 100

1. Theoretical yield: ----------gm.

2. Practical yield: ----------gm.
3. Percentage yield: ----------%
Precautions:
1. Wear safety goggles at all times in the laboratory
2. Wear rubber or plastic gloved to protect your hands from the dyes.
3. The dyes used in this experiment should be handled with the utmost care since they will
dye the skin and clothing. Be careful to keep the dye powders and solutions off the desk
tops. Clean up any spills immediately.
4. Most dye materials are irritants to the skin, eyes, and respiratory system and may be toxic
by inhalation and ingestion. In the event of skin contact, wash the affected area well with
water.
5. Hydrochloric acid is corrosive and can cause severe burns to the skin along with irritating
fumes. Work with the concentrated solution under a hood. In the event of skin contact,
wash the affected area well with water. If the skin is broken or blistered, seek medical
assistance. If irritated by the vapors, get fresh air immediately.
6. Sodium hydroxide is caustic and can cause severe burns to the skin. Do not handle
sodium hydroxide pellets with your hands. In the event of skin contact, wash the affected
area well with water until there is no soapy feel. If the skin is broken or blistered, seek
medical assistance.
7. Sodium nitrite is an irritant to the skin, eyes, and respiratory system. It is toxic by
ingestion. In the event of skin contact, wash the affected area well with water. Sodium
nitrite can also be an explosion hazard. Do not heat this compound dry or in contact with
any flammable material.
8. Ammonia vapors are irritants to the eyes and respiratory system. Work with the

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concentrated solution under a hood. In the event of skin contact, wash the affected area
well with water. If irritated by the vapors, get fresh air immediately.

Quiz:
1. Solubility depends upon
a. temperature
b. solute
c. solvent
d. all of above
2. Medicinal drugs are bitter in taste hence they are added with
a. sugar
b. salt
c. water
d. dry ice
3. Some metals are so unreactive that they do not react with
a. copper
b. silver
c. gold
d. all of above
4. When a large amount of solute dissolves in a given amount of solvent it forms
a. dilute solution
b. saturated solution
c. aqueous solution
d. concentrated solution
5. Acid which is found in sting of a bee and bite of an ant is
a. carbonic acid
b. lactic acid
c. formic acid
d. citric acid
6. A dye or a mixture of dye which changes color according to acidity or alkalinity of any
substance is called

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a. indicator
b. pH scale
c. pH meter
d. balance scale
7. Maximum amount of solute which can dissolve in 100g of solvent at room temperature
is called
a. solubility
b. capacity
c. eligibility
d. tendency
8. If pH value is less than 7, nature is
a. acidic
b. basic
c. neutral
d. normal
9. A reaction in which an acid and alkali react together to form salt and water is called
a. chemical reaction
b. physical reaction
c. potential reaction
d. heat reaction
10. Zero is percentage of solubility of salt in
a. water
b. alcohol
c. acid
d. base

Marks: Signature:
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Experiment No.: …10.. Date: ………..

Preparation of fast green o dye
Objective: Preparation of fast green o dye.

Material Required:
Resorcinol, Sodium chloride, sodium nitrite, HCl acid etc.

Theory:
Disperse dyes are water insoluble non-ionic dyes used to dye man-made fibers from acidic
bath, specially designed for dyeing of polyester and are applied along with dispersing agent
to retain dyes in fine dispersion

Reaction:

Procedure:
Dissolve 10gm resorcinol in 100ml of water. Add 20cc HCl and 25gm NaCl in above

solution. Add ice and bring temperature to 0oC. Stir the solution mechanically. Prepare a

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solution of 13gm sodium nitrite in 50ml water. Allow nitrate solution to flow very slowly.
This takes about 60 minutes. When liquid show acidic nature, allow stand for one hour.
Filter the precipitate, wash with cold water and dry.

Result:
% yield = (Practical yield/ Theoretical yield) 100

1. Theoretical yield: ----------gm.

2. Practical yield: ----------gm.
3. Percentage yield: ----------%

Precautions:
1. Wear safety goggles at all times in the laboratory
2. Wear rubber or plastic gloved to protect your hands from the dyes.
3. The dyes used in this experiment should be handled with the utmost care since they will
dye the skin and clothing. Be careful to keep the dye powders and solutions off the desk
tops. Clean up any spills immediately.
4. Most dye materials are irritants to the skin, eyes, and respiratory system and may be
toxic by inhalation and ingestion. In the event of skin contact, wash the affected area
well with water.
5. Hydrochloric acid is corrosive and can cause severe burns to the skin along with
irritating fumes. Work with the concentrated solution under a hood. In the event of skin
contact, wash the affected area well with water. If the skin is broken or blistered, seek
medical assistance. If irritated by the vapors, get fresh air immediately.
6. Sodium hydroxide is caustic and can cause severe burns to the skin. Do not handle
sodium hydroxide pellets with your hands. In the event of skin contact, wash the
affected area well with water until there is no soapy feel. If the skin is broken or
blistered, seek medical assistance.
7. Sodium nitrite is an irritant to the skin, eyes, and respiratory system. It is toxic by
ingestion. In the event of skin contact, wash the affected area well with water. Sodium
nitrite can also be an explosion hazard. Do not heat this compound dry or in contact with
any flammable material.

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8. Ammonia vapors are irritants to the eyes and respiratory system. Work with the
concentrated solution under a hood. In the event of skin contact, wash the affected area
well with water. If irritated by the vapors, get fresh air immediately.

Quiz:
1. Wasp sting is neutralized by rubbing skin with
a. soap
b. orange juice
c. vinegar
d. anti acid
2. Solution which can hold no more solute is called
a. dilute solution
b. saturated solution
c. aqueous solution
d. concentrated solution
3. A common and universal solvent is
a. air
b. water
c. oxygen
d. nitrogen
4. In hydroponics, roots of a plant are immersed in solution of dissolved
a. mineral salts
b. fertilizers
c. chemicals
d. oxygen
5. Acid rain is
a. corrosive
b. damage living things
c. damage buildings
d. all of above
6. Alkaline has ph value above
a. 10
b. 14
c. 4
d. 7
7. Dilute acids form hydrogen gas when they react with
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a. reactive carbonates
b. reactive metals
c. oxides
d. amino acids
8. Solubility of a solid solute will increase with increase of
a. mass
b. volume
c. temperature
d. pressure
9. In dry form copper sulphate crystals and sodium hydroxide pellets
a. do no react
b. react vigorously
c. react slowly
d. dissolve completely
10. Liquid in which any salt gets dissolved is called a
a. solute
b. solvent
c. mixture
d. product
11. Elements in air that are responsible for acid rain include
a. oxides of nitrogen
b. sulphur dioxide
c. carbon dioxide
d. both a and b
12. Some acids react and burn skin if they come in contact with it. They are
a. corrosive
b. strong
c. light
d. both a and b
13. Nature of solute has an effect on its
a. solubility
b. reaction
c. distillation
d. purification
14. Color of concentrated copper sulphate solution appears
a. light blue
b. dark blue
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c. violet
d. indigo
15. Oranges and lemon are sour due to presence of
a. citrus acid
b. acetic acid
c. citric acid
d. carbonic acid
16. Tooth decay occurs in our mouth due to presence of
a. bacteria
b. virus
c. fungus
d. algae
17. Bee sting is acidic in nature which can be neutralized and made less painful by
applying
a. soap
b. lemon juice
c. vinegar
d. antacid
18. Number of factors on which solubility depends, is
a. 1
b. 2
c. 3
d. 4
19. When one or more solutes dissolve in a solvent they make a
a. solute
b. solvent
c. mixture
d. solution
20. A substance which has a bitter taste, soapy to touch and turns red litmus into blue is
called
a. alkali
b. acid
c. solution
d. solvent

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Marks: Signature

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