Department of Chemical Engineering, Veer Surendra Sai University of Technology

Process Technology
Lab Manual

List of Experiments

Sl. No. Name of the Experiment

1 To prepare soap and to determine the percentage yield of soap using a given oil
sample
2 To determine the alkali content of a given soap sample
3 To determine the partition co-efficient of Iodine between an organic solvent and
water
4 To determine the fat content in a given food stuff sample

5 To determine the ferrous iron concentration in Mohr’s salt solution using KMnO4

6 To determine the dye concentration using UV- visible spectrophotometer

 Department of Chemical Engineering, Veer Surendra Sai University of Technology

Experiment 1

Aim: To prepare soap and to determine the percentage yield of soap using a given oil sample

Apparatus required:

 Water heater bath

 Weighing balance
 Beaker: 250 cc
 Glass rod

Chemical required:

 Sunflower oil – 20 g
 About 3 cc of NaOH 25% (w/w)
 Na2CO3 – 4 g
 Na2SiO3 – 0.2 g
 NaCl – 0.4 g
 Water – 20 mL

Procedure:

1. Wash the beaker and dry it in hot air oven for 30 minutes
2. Take 20 g oil in the beaker
3. Fit the beaker in the insulating grip made up of thermocol
4. Add 6 mL of 25 % NaOH solution in beaker
5. Mix the contents thoroughly in the beaker with the help of a glass rod and keep it in a
water bath at a temperature of 230-250 F with continuous stirring
6. Add water (20 mL) to keep the mixture in liquid state
7. Add Na2CO3 (4 g) to complete saponification reaction
8. Cool the mixture at room temperature.
9. Add about NaCl (0.2 g) to separate the foam layer after completion of the saponification
reaction
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10. Add Na2SiO3 (0.2 g) and mix the contents.

11. Separate the soap from the mixture.

Calculation:

 Wt. of sunflower oil = 20 g

 Wt. of Na2CO3 = 4 g
 Wt. of NaCl = 0.2 g
 Wt. of Na2SiO3 = 0.2 g
 Wt. of water = 20 g
 Total wt. oil mixture = 44.4 g
 After soap formation, total wt. = X g
 Wt. of container = Y g
 Wt. of soap formed = (X-Y) g
 % yield of soap = (X-Y)*100/44.4

Result:

The percentage yield of soap of the given oil sample was found to be ---------.

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 Department of Chemical Engineering, Veer Surendra Sai University of Technology

Experiment 2

Aim: To determine the alkali content of a given soap sample

Apparatus required:

 Conical flask
 Beaker
 Separating funnel
 Glass rod
 Weighing balance
 Burette and Pipette

Chemicals Required:

 Diethyl ether
 NaCl (25 mL)
 H2SO4 (1N)
 NaOH (1N)
 Methyl orange indicator (4-6 drops)
 Distilled water

Procedure:

1. Weigh 5 g of soap sample accurately and transfer into a 250 mL beaker

2. Add 50 mL hot water to completely dissolve the soap
3. Add 4-6 drops of methyl orange indicator to the soap solution
4. Add 15 mL of 1N H2SO4 to the solution drop wise till the color changes from orange to
pink
5. Add 20 mL of diethyl ether to the mixture using a test tube
6. Transfer the mixture into a separating funnel to separate the bottom layer and collect
using a beaker
7. Add 25 mL of NaCl solution to the bottom layer and titrate with 1N NaOH solution
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 Department of Chemical Engineering, Veer Surendra Sai University of Technology

8. Record the initial burette reading

9. Add NaOH solution till the color of the solution changes from pink to orange
10. Note the final burette reading

Tabulation:

SL. No. Initial reading (IR) Final reading (FR) Difference

Calculation: (For sodium soap)

Total alkali content in mass percentage = [4.0*((V1*N1)-(V2*N2))]/M

V1 = volume of H2SO4 solution used in mL

V2 = volume of NaOH solution used in mL

N1 = Normality of H2SO4

N2 = Normality of NaOH

M = Mass in grams of soap in g

Tabulation:

Sl No Initial reading (IR), mL Final reading (FR), mL Difference

Result:-The alkali content of the given soap sample was found to be___________

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 Department of Chemical Engineering, Veer Surendra Sai University of Technology

Experiment 3

Aim: To determine the partition co-efficient of Iodine between an organic solvent and water

Apparatus required:

1. Stopper glass bottle

2. Separating funnel
3. Beakers: 4 no.
4. Conical flask: 2 no.
5. Measuring cylinder: 1 no.
6. Burette
7. Stand

Chemicals required:

1. Saturated solution of I2 in CCl4

2. Na2S2O3 solution (N/10 and N/100)
3. Starch solution
4. Potassium Iodide (KI)

Procedure (A):

1. Take four glass stopper bottles of about 150 mL capacity

2. Wash these bottles with water and allow drying. Name the bottles as No. 1, 2, 3 and 4
3. Add 50 mL of distilled water in each of these bottles and add the saturated solution of
iodine in benzene and benzene as per Table 1

Observation Table 1

Bottle no. Volume of Iodine in mL Volume of Benzene in mL

1 10 40
2 20 30
3 30 20

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4 40 10

Procedure (B):

1. Shake each bottle (closed) vigorously for 20 minutes (shaking of each bottle is necessary
for getting accurate results)
2. Keep these bottles undistributed for some time and allow to separate the two layers
3. Pour the contents of these bottles separately into a separating funnel and collect benzene
and water layers of each bottle in separately numbered beaker
4. Pipette out exactly 5mL of benzene layer from the separated layers of bottle no. 1 into a
conical flask
5. Add 1 g of potassium iodide and 5 drops of the starch solution
6. Do titration for the solution against (N/10) Na2S2O3 from the burette
7. Continue the titration, till the blue color get disappear
8. Repeat three times to get concordant readings
9. Repeat this process with benzene layers of other bottles also in the same manner
10. Pipette out 10 mL of aqueous layer of bottle no. 1 into a conical flask
11. Add 1 g of potassium iodide and 5 drops of the starch solution
12. Titrate this solution against (M/100) Na2S2O3 from the burette
13. Continue the titration till the blue color get disappear
14. Repeat three times to get concordant readings
15. Repeat this process with aqueous layers of other bottles in the same way
16. Note the room temperature using thermometer

Observation Table 2

Bottle Aqueous layers (C1) Benzene layers (C2)

number
Burette Reading in mL Burette Reading in mL
I.B.R F.B.R Volume Mean I.B.R F.B.R Volume Mean
used value used value
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 Department of Chemical Engineering, Veer Surendra Sai University of Technology

1. 1. 10 V1 5 V5
2.
3.
2. 1. 10 V2 5 V6
2.
3.
3. 1. 10 V3 5 V7
2.
3.
4. 1. 10 V4 5 V8
2.
3.

A) For Aqueous layer

Volume of aqueous layer taken for titration = 10 mL
Mean value of (N/100) Na2S2O3 solution = V1
10 mL of N1 iodine = V1 mL of (N/10) Na2S2O3
or N1 = V1 × (1/100) × (1/10) = (V1/1000)
Thus, the concentration of I2 in water layer = 127 × (V1/1000) gram equivalent / liter
(Since equivalent of I2 = 127) = C1
B) For Benzene layer
Volume of benzene layer taken for titration = 5 mL
Mean value of (N/10) Na2S2O3 solution = V5 mL
5mL of N2 iodine = V5 mL of (N/10) Na2S2O3
or N2 = V5 × (1/10) × (1/5) = (V5/50)
Thus the concentration of I2 in benzene layer = 127× (V5/50) gram equivalent/liter = C2

Partition co-efficient (K) = C1/ C2

= [127 × (V1/1000)]/ (127× V5/50)

= 127 × (V1/1000) × (50/127 × V5)

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= (V1 × 50)/ (V5× 1000) = (V1)/ (V5 ×20) -------------------------- (I)

The value of the partition coefficient (K) is calculated in the same way for other bottles
by using the simplified formulae as given under.
For bottle no. 2, K= C1/ C2= (V2)/ (V6×20)
For bottle no. 3, K= C1/ C2= (V3)/ (V7×20)
For bottle no. 4, K= C1/ C2= (V4)/ (V8×20)

The mean value of K obtained after using the relationships (I), (II), (III) and (IV) as given
above gives the value of the partition coefficient (K) of iodine between water and benzene.

Conclusion:

The partition co-efficient of iodine between benzene and water was found to be ____ at
___ oC.

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 Department of Chemical Engineering, Veer Surendra Sai University of Technology

Experiment 4

Aim: To determine the fat content of a given food stuff sample

Apparatus required:

 Soxhlet apparatus
 Weighing balance
 Thimble

Chemicals required:

 n-hexane
 Petroleum ether
 Ethanol
 Food stuff

Theory:

The fat or extractive content in food stuff can be extracted completely by using solvents
such as n-hexane, ethanol and petroleum ether

Description of Soxhlet apparatus:

The apparatus is consisting of three parts such as a round bottom flask, an extraction
section and a condensing section. A thimble filled with sample is placed in the extraction section.
The three parts of the apparatus are connected and placed over heating mental at a constant
temperature. Cold water is circulated in the condenser (top section of the apparatus) to condense
the evaporated solvent. The condensed solvents falls drop wise on the thimble where frequent
contact between the feed and the solvent occurs and the extractives get solubilized in the solvent.
The solution gets transfer to the round bottom flask after reaching a particular level above the
thimble. This process should be continued for 3 to 4 h to extract maximum soluble.

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Procedure:

1. Record the empty weight of the thimble (wo)

2. Ground the given peanuts (12 g) into very small size, place inside the thimble and note
the weight of the filled thimble accurately (w1)
3. Put the sample filled thimble in the extraction section of the Soxhlet apparatus
4. Fill the round bottom flask with the solvent (400 mL) and connect all the section of the
apparatus above a heating mental
5. Start the heating process at a constant temperature (boiling point of the solvent) and keep
circulating cold water in the condenser section
6. Continue the process of extraction for 3 h and observed the change in color of the
solution in the thimble section.
7. Stop the process of heating when no change in the color is observed.
8. Remove the thimble very carefully so that the sample remaining in the thimble will not
fall outside and then dry and weigh it accurately.
9. Note the final weight of the thimble is w2
10. Similarly, follow all the steps by taking different solvents to determine the removal
efficiency

Calculations:

% fat/extractives in the given sample = ((w1-w2)/ (w1-w0)) × 100

Conclusion:

The removal efficiency of fats/extractive from _____ sample was found to be ____ % using ____
solvent.

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 Department of Chemical Engineering, Veer Surendra Sai University of Technology

Experiment 5
Aim: To determine the ferrous iron concentration in Mohr’s salt solution using KMnO4

Chemicals required:

 Standard oxalic acid solution

 Sulphuric acid
 Potassium permanganate solution
 Ferrous ammonium sulphate
Apparatus required:
 Burette
 Pipette (10 mL)
 Beaker
 Conical flask
 Hot water bath
 Thermometer
Procedure:

Standardization of potassium permanganate

1. Rinse burette with water and with KMnO4 solution

2. Fill the burette with KMnO4 solution
3. Pipette out 10 mL of standard sodium oxalate solution into a conical flask
4. Add 10 mL of 2N H2SO4 solution to it
5. Heat this solution at 70 oC using a hot water bath for 15 minutes
6. Titrate the solution against KMnO4 from the burette till the solution becomes permanent
pink color
7. Repeat three times to get concordant readings

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Observation Table 1
No. of Volume of oxalic acid + volume of Burette reading in mL Remarks
obs. H2SO4 in mL IBR FBR Difference
1 10+10
2 10+10
3 10+10
4 10+10

Calculation:
Vol. of KMnO4 consumed (V1) = X mL
Vol. of oxalic acid (V2) = 10 mL
Strength of KMnO4 (S1) =
Strength of oxalic acid (S2) =
S1=V2*S2/V1
Estimation of iron:
1. Pipette out 10 mL of Mohr’s salt [FeSO4(NH4)2SO46H2O] solution into a conical
flask
2. Add 10 mL of (2N) H2SO4 solution to it
3. Titrate the solution against KMnO4 from the burette till the solution becomes
permanent pink color
4. Repeat the procedure to get three concordant readings

Observation Table 1

No. of Volume of Ferrous ammonium Burette reading in ml. Remarks

obs. sulphate + volume of H2SO4 in ml. IBR FBR Difference
1 10+10 rough
2 10+10
3 10+10
4 10+10

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 Department of Chemical Engineering, Veer Surendra Sai University of Technology

Calculation:
Strength of KMnO4 = Z
1000 ml of (1N) KMnO4 = 55.85 g of Fe+2 ion
Y ml of Z(N/10) KMnO4 = 55.85*Y*Z/(1000*10) = A g of Fe+2 ion
10 ml of supplied solution contains = A g of Fe ion
1000 ml of supplied solution contains = (A*1000)/(10) g of Fe+2 ion
= B*1000 mg of
= _____ mg of Fe+2 ion
Conclusion:

The amount of Ferrous iron present in the Mohr’s salt is _____ ppm.

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 Department of Chemical Engineering, Veer Surendra Sai University of Technology

Experiment-6

Aim: To determine the dye concentration using UV- visible spectrophotometer

Apparatus required:

 UV-visible spectrophotometer

 Volumetric flask

 Pipette

 Measuring cylinder

Materials required:

 Dye

 Distilled water

Theory:

Beer-Lambert’s law states that there is a linear relationship between the concentration

and the absorbance of the solution. The concentration of a solution can be calculated by

measuring the absorbance of the sample.

According to Beer's Law, A = εbc, where A is absorbance, ε is the molar absorptive with units

of L mol-1 cm-1 (formerly called the extinction coefficient) b is the path length of the sample,

usually expressed in cm and C is the concentration.

The molar extension coefficient is given as a constant for each molecule. The absorbance does

not carry any unit. Since the absorbance and path length is known the concentration of any

unknown sample can be determined.

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Procedure:

1. Prepare 100 mL of 0.001M KMnO4 standard stock solution

2. Prepare six standards in 100 mL volumetric flask with concentration of 0.0004M

(solution-1), 0.0002M (solution-2), 0.0001M (solution-3), and 0.00005M (solution-4) by

diluting the stock solution prepared in step-1

3. Rinse one cuvette with distilled water and fill with water

4. Put the cuvette in the sample compartment of UV-visible spectrophotometer. This is the

reference solution.

5. Set the wavelength to 400 nm and set the absorbance to zero

6. Rinse the second cuvette once with distilled water and once with standard solution-

1(0.001M) KMnO4

7. Then fill the standard solution 1 in the cuvette

8. Place the cuvette in the sample compartment and measure the absorbance at 410 nm

9. Repeat the procedure (step-3 and 4) above for the two cuvette as wavelength

420,440,450, 500, 550, 600 nm.

10. Sett the absorbance to 0 for the cuvette with water .measure absorbance for the cuvette

with 0.001M KMnO4 and record the absorbance at each wavelength in the data Table

11. Prepare a graph of absorbance (A) vs. wavelength λ and determine the maximum

wavelength (λ)

12. Check the maximum λ in the UV visible software. Place the cuvette with the distilled

water in the same compartment and again set the absorbance to zero. Measure and

record the absorbance of each of 6 standard solutions starting with the most dilute

standard. After each measurement rinse the cuvette with next standard not with the
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distilled water. Draw a plot having x-axis as concentration in moles/lit and y-axis as

absorbance at maximum λ

13. Using Beer-Lambert’s law to calculate the concentration £ for KMnO4 by assuming the

width of cell or path length to be 1cm.

Observation Table 1

Solution Concentration of solution (in M) Volume of stock solution added in mL

1 0.0004M

2 0.0002M

3 0.0001M

4 0.00005M

Observation Table 2

Concentration Absorbance

430nm 440nm 450nm 500nm 600nm

0.0004M

0.0002M

0.0001M

0.00005M

Absorbance of different concentration KMnO4 at different λ has to be performed to determine

the maximum absorbance of KMnO4 solution. Then plot a graph of absorbance Vs wavelength.

Conclusion: The concentration of unknown sample was found to be_____

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