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CHEMICAL PROCESSING LABORATORY MANUAL
B.Tech II Year / I Semester
COURSE CODE: CH206

Chemical Processing Laboratory Page 1
List of Experiments
I. Analysis:
Soap:
Experiment 1a: Alkali content
Experiment 1b: Fatty acid content
Edible Oil:
Experiment 2. Acid Value
Experiment 3. Peroxide Value
II. Product Synthesis:
Experiment 4: Preparation of Soap
III. Testing Methods of fuels:
Experiment 5: Flash and Fire point
Experiment 6: Aniline point
IV. Mechanical Operations:
Experiment 7: Ball mill
Experiment 8: Screen Effectiveness
Experiment 9: Sedimentation
Experiment 10: Vapour-Liquid Equilibrium Setup

Analysis of Soap
Experiment 1a: Fatty acid content
AIM: To determine the fatty acid content present in the given sample of soap.
PRINCIPLE: Soaps are metallic salts of high molecular weight, linear chain, and mono-
carboxylic acids. They are water-soluble. In acid medium soaps are converted into its fatty
acid.They are insoluble in water at cold conditions. These insoluble fatty acids may separate and
gives the total fatty matter of soap.
REAGENTS REQUIRED: Soap Sample, 0.5N HCl solution,NaOH solution, Phenolphthalein.
APPARATUS REQUIRED: Measuring cylinder, Burette 50 ml, Beaker 100 ml, conical flask 250ml,
heating water bath, Whatman 41 filter paper
PROCEDURE:
TITRATION
ESTIMATION OF FATTY CONTENT
5g of soap sample is taken in a conical flask and it is dissolved in 100ml of warm water to give
homogeneous solution. 100ml of makeup solution is taken in a beaker and 40ml of 0.5N hydrochloric
acid is added. It is allowed to heat in a water bath for 30minutes and cooled. It is filtered using
Whatman 41 filter paper. The precipitate is initially dried and weighed (𝑚1 𝑔𝑟𝑎𝑚𝑠). Then 20 ml of
isopropyl alcohol is added to the dried precipitate and also add phenolphthalein indicator. It is titrated
against 0.5N sodium hydroxide. The end point is the appearance of pink color.
TABULATION:
TITRATION
ESTIMATION OF FATTY ACID CONTENT
End Point: Appearance of pink color Indicator: Phenolphthalein
S.No
Burette Reading (ml) Volume of
NaOH(ml)
Initial (ml) Final(ml)
1

CALCULATION:
W𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑑𝑟𝑦 𝑝𝑟𝑒𝑐𝑖𝑝𝑖𝑡𝑎𝑡𝑒 = 𝑚1 𝑔𝑟𝑎𝑚𝑠
% 𝑡𝑜𝑡𝑎𝑙 𝑓𝑎𝑡𝑡𝑦 𝑎𝑐𝑖𝑑 , 𝑒𝑥𝑝𝑟𝑒𝑠𝑠𝑒𝑑 𝑎𝑠 𝑚𝑎𝑠𝑠 =
𝑉 is number of ml of NaOH used
𝑁 is exact normality of NaOH
𝑚 is mass in grams of sample soap (2 grams)
RESULT:
[𝑚1 − (0.022 × 𝑁 × 𝑉)] × 100
𝑚
MECHANISM &REACTIONS INVOLVED:
DISCUSSION:

Experiment 1b: Alkali content
AIM: To determine the alkali content present in the given sample of soap.
PRINCIPLE: Soaps are metallic salts of high molecular weight, linear chain, and mono-
carboxylic acids. They are water-soluble. In acid medium soaps are converted into its fatty acid,
they are insoluble in water at cold conditions. These insoluble fatty acids may separate and gives
the total fatty matter of soap.
REAGENTS REQUIRED: Soap Sample, 0.5N HCl solution, NaOH solution, isopropyl alcohol,
Phenolphthalein.
APPARATUS REQUIRED: Measuring cylinder, Burette 50 ml, Beaker 100 ml, conical flask 250
ml, heating water bath, Whatman 41 filter paper
PROCEDURE:
TITRATION:
ESTIMATION OF ALKALI CONTENT
5g of soap sample is dissolved in 100ml of warm water to give homogeneous solution. 100ml of
this solution is taken in a beaker and 40ml of 0.5N hydrochloric acid is added and allowed to heat
for 30 minutes in a water bath. Then the solution is cooled. After cooling it is filtered using
Whatman 41 filter paper. The filrate and precipitate are separated. The complere filtrate has to be
taken in a conical falsk and add few drops of Phenolphthalein indicator and titrate against 0.5N
NaOH. The end point is the appearance of pink color. From the filtrate, 20ml of the solution is
taken in a conical flask and 2 drops of Phenolphthalein indicator is added. It is titrated against 0.5N
NaOH. The end point is the appearance of pink color
TABULATION:
TITRATION:
ESTIMATION OF ALKALI CONTENT
S.No
NaOH(ml)
1

CALCULATION:
Sodium Soap:
4.0 × [(𝑉1 × 𝑁1) − (𝑉2 × 𝑁2)]
𝑇𝑜𝑡𝑎𝑙 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 , 𝑒𝑥𝑝𝑟𝑒𝑠𝑠𝑒𝑑 𝑎𝑠 𝑎 𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 = [ ]
𝑚
Potassium Soap:
5.6 × [(𝑉1 × 𝑁1) − (𝑉2 × 𝑁2)]
𝑇𝑜𝑡𝑎𝑙 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 , 𝑒𝑥𝑝𝑟𝑒𝑠𝑠𝑒𝑑 𝑎𝑠 𝑎 𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 = [ ]
𝑚
𝑉1 is the number of ml of the HCl acid solution is added to the soap solution ( 40 ml)
𝑉2 is the number of ml of the NaOH solution used
𝑁1 is the exact normality of HCl solution
𝑁2 is the exact normality of NaOH solution
𝑚 is mass in grams of sample soap (2 grams)
RESULT:
MECHANISM &REACTIONS INVOLVED:
DISCUSSION:

Analysis of Edible Oils
Experiment 2: Acid Value
Aim: Estimation of acid value for given edible oil.
PRINCIPLE: Acid value is defined as the amount of potassium hydroxide in milligrams required to
neutralize the free fatty acids present in one gram of oil/fat. It is a respective measure of rancidity as free
fatty acids which are normally formed during decomposition of oil glycerides. 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.
REAGENTS REQUIRED:
1. Oils and fats
2. Phenolphthalein indicator solution
3. Ethyl alcohol: Ninety-five percent alcohol neutral to Phenolphthalein indicator.
4. Standard aqueous Potassium hydroxide or sodium hydroxide solution 0.1 N.
APPARATUS REQUIRED: 1. General Glass ware and apparatus, Ambered colored bottle, Brown
glass bottle
PROCEDURE:
Titration: Estimation of Acid Value
Mix the oil or melted fat thoroughly before weighing. Weigh accurately 5 g of the cooled oil sample in
a 250 mL conical flask. Add 50 mL of freshly neutralised hot ethyl alcohol and about one ml of
phenolphthalein indicator solution. Heat the mixture for about fifteen min in water bath (75-80 °C).
Titrate while hot against standard alkali solution shaking vigorously during the titration. End point using
phenolphthalein indicator shall be from colorless to light pink (Persisting for 15 sec.).

TABULATION
S.No
Alkali (ml)
1
CALCULATION:
W
56.1
*
N
*
V
=
acids
fatty
of
g
per
KOH
mg
value,
Acid
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 g of the sample
Acid value = % fatty acid (as oleic) x 1.99

Experiment 3: Peroxide Value
Aim: Estimation of peroxide value for given edible oil.
PRINCIPLE:
Detection of peroxide gives the initial evidence of rancidity in unsaturated fats and oils. It gives
a measure of the extent to which an oil sample has undergone primary oxidation where extent of
secondary oxidation may be determined from p-anisidine test.
Natural oils and fats are susceptible to deterioration due to rancidity. The major cause of rancidity
is oxidation. Autoxidation is the most common process. The process is generally accelerated at elevated
temperatures, exposure to sunlight etc. The other form is thermal oxidation that may occur during deep
frying. Unsaturated fatty acids are the most susceptible to these reactions whether these are in free-state
or bound to the glyceride moiety. This reaction is believed to occur via a free radical chain reaction. This
reaction proceeds through the following three steps: initiation, propagation and termination.
Oxidation generally proceeds very slowly at the initial phase and suddenly the reaction rate
becomes very fast. This period taken to reach the sudden increase in reaction rate is referred to as
induction period. Hydroperoxides are produced as the primary oxidation product in autoxidation process.
These hydroperoxides are then decomposed to aldehydes, ketones, alcohols, hydrocarbons, volatile
organic acids and epoxy compounds. These are known as secondary oxidation products. These
compounds and the free radicals formed form the basis for estimation of the oxidative deterioration of
lipids.
Peroxide Value (PV) is a measure of total hydroperoxide content in the oil or fat sample. This is
the most important quality indicators of oils and fats during production and storage. This is an indicator
of initial stages of oxidative degradation. One can assess the quality of oil by determining the
hydroperoxide concentration over a period of time.
REAGENTS REQUIRED:
1. Oils/fats
2. Acetic acid-Chloroform Mixer (Mix 3 volumes of glacial acetic acid with 2 volumes of chloroform)
4. Potassium iodide (Saturated potassium iodide solution- about 10 g in 6 ml of water)
5. Sodium thiosulphate (0.01 N)
6. Potassium dichromate

7. Starch (1% water-soluble starch solution)
APPARATUS REQUIRED: 1. General glassware and apparatus, 2. Mohr‘s pipette
PROCEDURE:
Titration: Estimation of Peroxide Value
Weigh 5 g (±50 mg) sample into a 250 mL stoppered conical flask. Add 30 mL acetic acid chloroform
solvent mixture and swirl to dissolve. Add 0.5 mL saturated potassium iodide solution with a Mohr‘s
pipette. Let stand for one min in dark with occasional shaking, and then add about 30 mL of water. Add
about 0.5 mL starch solution as indicator and immediately titrate with sodium thiosulphate (0.1 N) to
release all I2 from chloroform layer until blue color disappears. If less than 0.5 mL of 0.1 N sodium
thiosulphate is used repeat using 0.01 N sodium thiosulphate. Conduct blank determination (must be less
than 0.1 mL 0.1 N sodium thiosulphate).
TABULATION
S.No
Burette Reading (ml) Volume of Sodium
Thiosulphate (ml)
1
2
CALCULATION:
g
sample,
the
of
Weight
1000
*
N
*
S)
-
(B
=
mg/Kg
value,
Peroxide
Where,
B = mL of Sodium Thiosulphate used (blank corrected)
S= Volume (mL) of Sodium Thiosulphate consumed for the sample
N = Normality of sodium thiosulphate solution.
Fresh oils usually have peroxide values well below 10 meq/kg. A rancid taste often begins to be
noticeable when the peroxide value is above 20 meq/kg (between 20 – 40 meq/Kg). In interpreting
such figures, however, it is necessary to take into account the particular oil or fat.

Experiment 4: Preparation of soap
AIM: Preparation of soap using edible oil as raw material
EQUIPMENT:
 Material Safety Data Sheets (MSDS) for Sodium Hydroxide and Ethyl Alcohol
 Latex gloves - 400 mL beaker
 100 mL graduated cylinder - hot plate
 30 g fat or oil - 15 mL of 50% NaOH solution
 30 mL ethyl alcohol
 200 mL saturated NaCl solution
CAUTION: Sodium hydroxide is a strong base and corrosive. Ethyl alcohol is flammable. Read
the appropriate MSDS in the lab for further information. Wear latex gloves and goggles during the
lab to protect yourself from the sodium hydroxide.
PROCEDURE:
1. Weigh 5ml of fat or oil into a 500 mL beaker. Record the exact amount.
2. Add 30 mL of ethyl alcohol and 15 mL of 50% NaOH solution.
Stir the mixture constantly with a glass stirring rod and heat gently (medium heat) on a hot plateuntil
the alcohol evaporates. (~30 min.). Do not allow your soap to boil.
3. Fill the beaker with a saturated salt solution (NaCl) and stir vigorously to "salt out" the soap.
4. Filter the soap and then take the wet and dry weight.
RESULT: The weight of the soap precipitate g (wet)
The weight of the soap precipitate g (dry)

Experiment 5: Flash and Fire point
AIM: To determine flash and fire point of liquid petroleum products by clove land open cup
method.
REQUIREMENTS: Clove land open cup apparatus, thermometers, beaker, petroleum sample.
THEORY: It is the lowest temperature at which the oil gives of vapor that will ignite where a
flame is passed over surface of the oil.
PROCEDURE: Clean and dry the brass cup. Fill the cup with the sample exactly to the mark
inside the cup. Adjust the micro flame. Heat the cup slowly at controlled rate at 3 °C per min. Pass
the micro flame across the cup for every rise of 3 °C of temperature. Record the lowest temperature
at which flame flash is observed at any point over the liquid. For determination of the fire point
continuous the heating of the sample of a controlled rate. Pass the test flame across the entire of
the cup for every degree in temperature rise.
OBSERVATION TABLE:
S.No Sample Flash point (°C) Fire point (°C)
1
2
3
RESULT:

Experiment 6: ANILINE POINT
AIM: To determine the aniline point of petroleum product and hydro carbon solvents.
REQUIRMENTS: Aniline point apparatus, thermometer, electrical heating devise, pipette.
THEORY: Definition of aniline point is the lowest temperature at which the sample is completely
miscible with equal volume of aniline. The value gives an approximation for the content of aromatic
components in the oils since the miscibility of the aniline which is also an aromatic compound suggests
that presence of similar (iearomatic compounds) in the oil. The lower aniline point greater is content of
aromatic compoundin the oil as obviously a lower temperature needed to ensure miscibility. The aniline
point serves as an proxy chemical oil largely consists of saturated hydrocarbons or unsaturated (mostly
aromatic only).
PROCEDURE: Clean and dry the apparatus. Add 20 ml of distilled aniline and 20 ml of given
sample it can be observed the formation of two layers. Arrange the apparatus with stirrer in such
a way that liquid in u tube and paraffin’s of the beaker are stirred simultaneously. Switch on heater
to heat the paraffin at a controlled rate so there is so much difference in the temperature of paraffin
bath and u tube. The minimum temperature at which two layers give the single phase is noted as
aniline point. Nowstirring at u tube mixture is stopped and mixture is allowed to cool. Temperature
at which two layers are formed is considered for mix aniline point. The above procedure is repeated
for courantevalue and changing the feed.
OBSERVATION:
1. Volume of aniline = 20 ml
2. Volume of kerosene = 20 ml
3. Cloud formation temperature = °C
4. One phase temperature = °C
5. Two phase formation temperature = °C
RESULT: Aniline point of the given sample °C

Experiment 7: BALL MILL
AIM:
To estimate the reduction ratio of a ball mill for a particular feed size and also to estimate the
critical and optimum speed for the operation of the ball mill.
FORMULAE REQUIRED:
1. Average feed diameter =
(D1+D2)
2
(mm)
D1 is the diameter of the large feed particle
D2 is the diameter of the small feed particle.
2. Average product diameter =
1
∑ xi/Davg
(mm)
xi is the mass fraction
Davg is the average diameter
3. Reduction ratio =
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑓𝑒𝑒𝑑 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟
4. Critical speed of mill, 𝜂𝑐 =
60
2𝜋
× √
𝑔
𝑅−𝑟
R – Radius of the mill
r – Radius of the ball
g – Acceleration due to gravity.
5. Optimum speed of the mill, ɳo = 60% of the critical speed.
THEORY:
It works on the principle of impact, i.e. size reduction is done by impact as the balls drop from
near the top of the shell. As the shell rotates, the solid particles in between the balls are ground and
reduced in size by impact. The mill contains various ages and sizes of balls. As the shell rotates,
the larger balls segregate near the feed end and small balls segregate near theproduct/discharge.
The initial breaking of the feed particles is done by largest balls and small particles by the small
balls. If the rate of feed is increased, the coarser product will be obtained and if the speed of the
rotation is increased (less than critical speed), the fineness for a given capacity increases. Optimum
grinding conditions are obtained when the volume of balls is equal to 50% that of the mill. For an
effective grinding, the ball mill should be operated at a speed (optimum speed) equalto 50 to 75%
of the critical speed.

After Size Reduction
Number of balls = Time = Speed =
S.No. Mesh
number
Mesh
opening
Davg Weight
retained
Mass
fraction
xi
xi/Davg Cummulative
mass fraction
ASTM mm mm mm - mm-1
PROCEDURE:
1. Feed of about 100 grams is weighed for first run.( Feed Size has to be measured)
2. 10 steel balls are taken along with the feed and introduced into the cylinder and closed
tightly.
3. The motor is allowed to run for 20 minutes.
4. Then the crushed product is sieved in given mesh order.
5. The same procedure is repeated where the motor is allowed to run for 20 minutes.
6. By this reduction ratio is calculated.
7. Then critical speed is calculated by theoretical formula.
RESULT:
Thus the given ball mill has been analyzed for reduction ratio, critical speed and optimum speed
Critical speed, ɳc = Optimum
speed, ɳo =Reduction ratio =
MODEL GRAPH:

EXPERIMENT 8 : SCREEN EFFECTIVENESS
Aim : To determine the screen effectiveness of the given screen.
Theory: Screening is the method of separating particles according to size alone. Standard screens are used to
mesh, the dimensions of which are carefully standardized. The openings are square. Each screen is identified
by the number of openings per linear inch. The actual openings are smaller than those corresponding to the
mesh numbers. One of the standard screen series is Tyler standard screen series. This set of screens is based on
the opening of the 200mesh screen, which is established at 0.074mm. The area of the openings in any one
screen in the series is exactly twice that of the openings in the next smaller screen is √2
In industrial screening the solids are dropped on, or thrown against, a screening surface. The undersize,
or fines, pass through the screen openings, oversize, or tails, do not. Industrial screens made from woven wire,
silk or plastic cloth, metal bars, perforated or slotted metal plates, or wires that are wedge shaped in cross
section. The effectiveness of a screen often called screen efficiency is a measure of the success of a screen in
closely separating oversize material, A and undersize material, B. If the screen functioned perfectly, all of
material A would be in the overflow and all of material B would be in the underflow. Effectiveness based on
the oversize material, EA is the ratio of oversize material A that is actually in the overflow to the amount of A
entering with the feed. Similarly, an effectiveness based on the undersize material, EB is the ratio of undersize
material B that is actually in the underflow to the amount of B entering with the feed. The overall effectiveness
is the product of the EA and EB.
PROCEDURE:
 A set of standard sieves were arranged serially in a stack with the smallest at
the bottom and the largest at the top.
 250g of sample was placed on the top screen and the stack was shaken for a
definite time.
 Particles retained on each screen were removed and weighed.
 The oversize and undersize particles were separated.
 The overflow analysis was performed using oversize particles and underflow
analysis was performed using undersize particles.
 The results of sieve analysis were tabulated.
 Screen effectiveness was calculated by using formula and graphically

f
f
FORMULAE:
1. Overall screen effectiveness E= EA.EB =
1. Overall screen effectiveness E= EA.EB =
x  x

B
x  xf
x xD 1 xB 
x  xB 2
x 1 x 

Where,
E = Overall screen effectiveness
EA = Effectiveness based on the oversize particle
EB = Effectiveness based on the undersize particle
xf = Cumulative mass fraction of oversize particle in feed
xD = Cumulative mass fraction of oversize particle in overflow
xB = Cumulative mass fraction of oversize particle in underflow
MODEL GRAPH
D
D f

TABLE 1:
Feed Overflow Underflow
S.No. M
es
h
No
.
Size
of
screen
openi
ng
(mm)
Mass
retain
ed (g)
Mass
fracti
on, xi
Cum.
Mass
fracti
on,
Mass
retain
ed (g)
Mass
fracti
on, xi
Cum.
Mass
fracti
on,
Mass
retain
ed (g)
Mass
fracti
on, xi
Cum.
Mass
fracti
on,
1
2
3
4
5
6
7
8
9
1
0
RESULT:
The screen effectiveness of the given screen..................... mm was found to be
---------------------- and graphically …………………………..

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