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Laboratory Manual- Mass Transfer Operations-I

EXPERIMENT NO:

SINGLE STAGE LEACHING


Aim: To determine the efficiency of single stage leaching experiment for leaching of NaOH and
CaCO3.

Apparatus: Glass beakers, glass rod, measuring cylinder and stirrer.

Chemicals: NaOH, CaCO3, Phenolphthalein and water.

Procedure:

 Clean all apparatus with water.


 Prepare the mixture for extraction by mixing 5 gm NaOH and 35 gm CaCO3 and transfer it to
a beaker.
 Add 200 ml of water into the beaker and stir the solution for about 10 min.
 Allow the mixture to settle and a clear liquid layer will form at the top, this is the extract
layer.
 Take 25 ml of the clear solution and titrate it against 0.5 N HCl with phenolphthalein
indicator.
 Note down the observation and do the calculation.

Observation:

1. Weight of feed NaOH -


2. Weight of feed CaCO3 -
3. Weight of solvent (water) -
4. Volume of clear solution -
5. Indicator -
6. Volume of extract -
7. Titrate reading -
8. Normality of HCl solution -

Calculation:

N2V2
i. For clear solution normality , N1=
V1

ii. Amount of NaOH in clear solution (extract)

= N1 × volume × gm equivalent of NaOH

Chemical Engineering Department, Government Engineering College, Bhuj


Laboratory Manual- Mass Transfer Operations-I

NaOH in clear solution (extract )


iii. % efficiency of leaching =
NaOH in feed

Result:

1.) NaOH in clear solution =


2.) % recovery of NaOH =

Conclusion:

Chemical Engineering Department, Government Engineering College, Bhuj


Laboratory Manual- Mass Transfer Operations-I

EXPERIMENT NO:

CRYSTALLIZATION

Aim: To study Crystallization & find crystal yield ‘with Seeding ’ & ‘ without Seeding ’.

Apparatus: Heating Mantle, Heater, Thermometer, Weigh scale, Vacuum filter, drying apparatus.

Chemicals: Boric acid crystal and Water.

Procedure:

 Without Seeding:

 Take 100 ml of water in beaker, heat it till 60° C.


 Add 15 gm Boric acid crystals and allow it to dissolve and mention temperature at 60° C up
to 15 minutes.
 Allow the solution to cool, wherein the crystals of Boric acid will start forming.
 Filter the crystals from the liquid and allow it to dry.
 Weight the crystals formed.

 With Seeding:

 Take 100 ml of water in beaker, heat it till 60° C.


 Add 15 gm Boric acid crystals and allow it to dissolve and mention temperature at 60° C upto
15 minutes.
 For Crystallization ‘with Seeding’ dissolve 5 gm of boric acid when the solution starts to cool
and crystallization starts.
 Filter the crystals from the liquid and allow it to dry.
 Weight the crystals formed.
 Calculate crystal yield ‘with Seeding’ & ‘without Seeding’.

Observations:-

1. Room temperature -
2. Test Temperature -
3. Wt. of Crystal obtained theoretically
a) Wt. of Crystal without seeding - ______________

b) Wt. of Crystal with seeding - ______________

Chemical Engineering Department, Government Engineering College, Bhuj


Laboratory Manual- Mass Transfer Operations-I

Calculation:-

1) % Yield without Seeding

Wt of Boric acid crystals collected


=
Wt of Boric acid crystals added

2) % Yield with seeding

Wt of Boric acid crystals collected


=
Wt of Boric acid crystals added

Result:-

1. Crystal yield without seeding - __________________


2. Crystal yield with seeding -__________________

Conclusion:-

Chemical Engineering Department, Government Engineering College, Bhuj


Laboratory Manual- Mass Transfer Operations-I

EXPERIMENT NO: -

MULTISTAGE LEACHING

Aim: To determine the efficiency of multistage leaching of NaOH & CaCO3 using water as solvent.

Apparatus: -Glass beakers, Magnetic stirrer, Burette, Pipette, Measuring cylinder and Conical flask.

Chemicals: 35gm CaCO3, 5gm NaOH, 0.5N HCl , water and phenolphthalein

Procedure: - .

 Clean all apparatus with water.


 Mix 5gm NaOH & 35gm CaCO3 and take it in a beaker.
 Add to it 195ml of water and stir the solution for about 10 min .
 Separate the clear solution from the top of the beaker and measure its volume.
 Take 25ml from collected clear solution and titrate it against 0.45N HCl solution with
phenolphthalein indicator.
 Now repeat the whole procedure after adding 195 ml of water to the sludge/slurry.
 Record the observations for the 2nd stage.

Observation: -

1. Weight of CaCO3 - __________


2. Weight of NaOH - __________
3. Volume of solvent water - __________
4. Volume of clear solution - __________
5. Indicator - __________

Calculation:

Stage 1:

N2V2
i. For clear solution normality , N1=
V1

Chemical Engineering Department, Government Engineering College, Bhuj


Laboratory Manual- Mass Transfer Operations-I

ii. Amount of NaOH in clear solution ( gm )

= N1 × volume × gm equivalent of NaOH

NaOH in clear solution


iii. % efficiency of 1st stage leaching =
NaOH added in feed

Stage 2:

N2V2
iv. For clear solution normality , N1=
V1

v. Amount of NaOH in clear solution (gm)

= N1 × volume × gm equivalent of NaOH

vi. Total amount of NaOH recovered in both stages =


( Sum of NaOH calculated in step ii and step v)

Total NaOH recovered in both stages


vii. % efficiency after 2nd stage leaching =
NaOH in feed

Chemical Engineering Department, Government Engineering College, Bhuj


Laboratory Manual- Mass Transfer Operations-I

Result:

1.) % recovery of NaOH in 1st stage -


2.) % recovery of NaOH after 2nd stage -

Conclusion:

Chemical Engineering Department, Government Engineering College, Bhuj


Laboratory Manual- Mass Transfer Operations-I

EXPERIMENT NO:

SINGLE STAGE EXTRACTION

Aim:-To determine the performance of single stage extraction of acetic acid and water mix with ethyl
acetic as solvent at room temperature.

Apparatus:-Measuring cylinder, Separating funnel, Magnetic stirrer, Conical flask, Burette stand,
Weight box etc.

Chemicals:-Water, Acetic acid, ethyl acetate, Phenolphthalein.

Procedure:-

 Clean all the apparatus with water.


 Take 50 ml water, 20 ml acetic acid, and 50 ml ethyl acetate in 250ml beaker.
 Stir mix for 30 min using stirrer.
 After stirring pour the mix in separating to two refers.
 Collect the two layers in two beakers.
 The upper layer is ethyl acetate extract layer.
 The lower layer of water is raffinate layer.
 Measure the volume and weight of the extract and raffinate the layer.
 Take 5ml extract layer and 2-3 drops of phenolphthalein and titrate against 0.5N NaOH.
 Note down the burette reading and calculate the efficiency of single stage extraction.

Observation:-

1. Volume of H2O -______


2. Volume of Benzene - ______
3. Volume of Acetic acid - ______
4. Volume of upper layer -_______
5. Volume of lower layer - ______
6. Weight of upper layer - ______
7. Weight of lower layer - ______
8. Titration reading (L.L) - ______
9. Normality of NaOH - ______

Calculations:-

N2V2
(1) Normality of extract , N1=
V1

Chemical Engineering Department, Government Engineering College, Bhuj


Laboratory Manual- Mass Transfer Operations-I

(2) Wt of Acetic Acid taken initially = Density x Volume

(3) Wt of Acetic Acid in extract = N1 x Vol. x gm equivalent of Acetic Acid

NaOH recovered
(4) % Recovery of Acetic Acid =
NaOH in feed

Result: - % Recovery of Acetic Acid =______

Conclusion:

Chemical Engineering Department, Government Engineering College, Bhuj

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