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AMAL JYOTHI COLLEGE OF ENGINEERING

KOOVAPALLY P.O., KANJIRAPALLY

DEPARTMENT OF CHEMICAL ENGINEERING

LABORATORY MANUAL
for
CH 010 708 MASS TRANSFER OPERATIONS LAB
Prepared by
Jayasree P K
Assistant Professor (Head-in-Charge)
Department of Chemical Engineering

Deepak Roy George


Assistant Professor(Faculty in Charge)
Department of Chemical Engineering

Reethu Sebastian
Lab Instructor Grade II
Department of Chemical Engineering
CONTENT
Exp NAME OF EXPERIMENT PAGE
No. NO.
1. Simple Leaching-I 1

2. Simple Leaching-II 4

3. Counter Current Leaching 8

4. Adsorption Isotherm 14

5. Batch Drying 20

6. Simple Distillation 23

7. Liquid Liquid Diffusion 29

8. Vapour in Air Diffusion 33

9. Steam Distillation 39

10. Cross Current Leaching 44

11. Absorption In Packed Bed 49

12. Packed Bed Distillation Column 57

13. Ternary Liquid Equilibrium 61


SIMPLELEACHINGI

AIM
To draw the percentage actual recovery vs solvent to feed ratio curve for singlestageleaching and
to compare actual recovery with theoretical recovery

APPARATUS&CHEMICALS REQUIRED
Beaker 500ml(6nos), pipette 20ml(l), 10ml(l), burette (50ml),volumetric flask 100ml(1) conical
flask(250ml),sand ,sodium carbonate, 0.1N HCl

PRINCIPLE
The method of separating one constituent from a solid or liquid mixture using a liquid solvent is
based on two methods. If the soluble component is dissolved from its mixture with an insoluble
solid the operation is called leaching or solid extraction.

The mixture of insoluble carrier solid and the solute to be extracted is called feed. The feed is
contacting with the solvent and the mixture is separated in to two streams. The solvent rich
product of operation is called the over flow or extract and the stream in which contains the bulk of
carrier solid is called leached solids or under flow and the unit of equipment in which operation
is carried out is called a stage. In simple batch operations if sufficient amount solvent is used, all
the solute can approximately get dissolved in the solvent. The amount of solute that is extracted
based on the assumption is called theoretical recovery. Leaching techniques can be classified as
batch wise and continuous.

PROCEDURE
Standardisation of HCl
Standardize the given HCl solution using N/10 Na2CO3 solution using 100ml volumetric flask.
Feed Preparation
10%by weight Na2CO3 and sand mixture is prepared by dissolving 45gms sand and 5gms
Na2CO3in 50cc distilled water.
Single Stage Varying Solvent Ratio
Different feed samples are prepared in the beakers. 50ml water is again added to beaker1 and the
mixture is allowed to settle after stirring. The amount equal to the amount of solvent added is
taken out in a measuring jar and 10ml of this solution is pipette out and diluted in to 100ml.From
this dilute 100ml solution, pipette out 10ml and titrate against standard HCl solution. The solvent
to feed ratio by volume is on sand free basis. The experiment is repeated using
100,150,200,250ml solvent in the remaining beakers and 20,30,40,50ml respectively of extract is

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pipette out after stirring and is made up to 100ml. 10ml of this solution is then titrated against
standard HCl solution.

The graph, percentage recovery both theoretical and actual versus solvent to feed ratio are drawn.

OBSERVATION

Beaker no Wt of Wt Of Volume of Volume of solvent


Na2CO3 sand water used
Solvent/feed ratio

Standardisation of HCl

Na2CO3 vs HCl Indicator :Methyl orange

Vol of Na2C03 Titre value 1 Titre value 2

Strength of extract: single stage

Beaker Extract used for Made upvolume Volume for titration Titre value
No. dilution

2
Single stage: varying solvent to feed ratio

BeakerNo. Normality of Solute extracted % actual recovery %theoretical recovery


extract

SAMPLE CALCULATION
Standardization of HCl
Wtof Na2CO3 =

Equivalent wt of Na2CO3 =

Normality of Na2CO3 = (wt/liter)/eq .wt =

Vol of HCl =

Normality of HC1 = (NNa2Co3* VNa2Co3)/ VHCL=

Single Stage; Varying Solvent to Feed Ratio

Normality of made up solution = (NHCI * VHCI)/ 10 =

Normality of extract = Normality of made up solution* dilution ratio=

Solute extracted = (Nextract* Equivalent wt of Na2CO3)*(V extract/1 000) =

%actual recovery =( solute extracted* 100) / Na2CO3 taken =

%theoretical recovery = (volume of extract* 100 )/ (volume of liquid when feed and solvent are
mixed)
RESULT
The percentage actual recovery vs solvent to feed ratio curve for single stage leaching has been
drawn.
INFERENCE

3
SIMPLE LEACHING-II

AIM
To draw the percentage actual recovery vs no of stages keeping the solvent to feed ratio constant
and to compare actual recovery with theoretical recovery

APPARATUS&CHEMICALS REQUIRED
Beakers500ml(6nos),pipette20ml(1),10ml(1),burette(50ml), volumetric flask 100ml(l) conical
flask(250ml),sand ,sodium carbonate, N/l0HCl

PRINCIPLE
The method of separating one constituent from a solid or liquid mixture using a liquid solvent is
based on two methods. If the soluble component is dissolved from its mixture with an insoluble
solid the operation is called leaching or solid extraction. The mixture of insoluble carrier solid and
the solute to be extracted is called feed. The feed is contacting with the solvent and the mixture is
separated in to two streams. The solvent rich product of operation is called the over flow or extract
and the stream in which contains the bulk of carrier solid is called leached solids or under flow and
the unit of equipment in which operation is carried out is called a stage. In simple batch operations
if sufficient amount solvent is used, all the solute can approximately get dissolved in the solvent.
The amount of solute that is extracted based on the assumption is called theoretical recovery.
Leaching techniques can be classified as batch wise and continuous. Experiment is conducted in
batch wise keeping the solvent to fed ratio constant.

PROCEDURE
Standardisation of HCl
Standardize the given HC1 solution using N/10 Na2CO3 solution using 100ml volumetric flask.
Feed Preparation
10% by weight Na2CO3and sand mixture is prepared by dissolving 45gms sand and 5gms Na2CO3 in
50cc water.
Batch Leaching for Constant Solvent to Feed Ratio
Different feed samples are prepared in five beakers; solute from each beaker is extracted with 200cc
of water but number of stages is varied from one to five. This is done as follows,to beaker No.l
200cc of water is added, then contents are well stirred ,the sand is allowed to settle and 200cc of
clear solution is pipetted out. From this 10ml is pipetted out and made up to 100ml using a standard
flask. Take 20ml from the made up solution .This is titrated against standard HCl using methyl
orange indicator.

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To beaker number 2,100cc of water is added and l00cc of clear solution is pipetted out in to a clean
beaker .Then, l00cc of fresh water is again added to the slurry and after mixing well,100cc of clear
solution is pipetted out and mixed with earlier extract. The strengths of new extract is found out by
titration against standard HCl

To beaker 3- Extracted 3 times using 66.6cc water in each time


To beaker 4- Extracted 4 times using 50cc water in each time
To beaker 5 – Extracted 5 times using 40cc water in each time
The graph is plotted for percentage recovery both theoretical and actual versus no of stages.

OBSERVATIONS

Beaker Wt of Wt of Water Volume of Solvent for No of Solvent/feed


no Na2CO3 sand ml extract each stage stages ratio

Standardisation of HCl

Na2CO3 Vs HCl Indicator :Methyl orange

Vol of Na2CO3 Titre value 1 Titre value 2

5
Extract Vs HCl Indicator :Methyl orange

Beaker Extract used for Made up Volume taken for Titre Vol of
no dilution volume titration value HCl

Beaker Normality of Solute extracted % actual % theoretical


extract recovery recovery
No

SAMPLE CALCULATION
Standardization of HCl
Wtof Na2CO3 =
Equivalent wt of Na2CO3 =
Normality of Na2CO3 = (wt/liter)/eq .wt =
Vol of HCl =
Normality of HC1 = NNa2Co3* VNa2Co3/ VHCL=
For Constant Solvent to Feed Ratio
Beaker No. 1

Normality of extract = (NHCI * VHCI) 100/(20*10) =

Solute extracted = (NEXTRACT* equivalentwt of Na22CO3)*(V EXTRACT/1 000) =

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% actual recovery = solute extracted* 100/ Na22CO3 taken =

% theoretical recovery = (vol of extract/ vol of liquid when feed and solvent are mixed)* 100 =
Beaker No. 2
Actual recovery is calculated as above
Theoretical recovery for lstStage= (100/(100+50))* 100=66.67%
Theoretical recovery for2ndStage= (1-0.667)*(100/(100+50))* 100 =22.7%

Total recovery =66.67+22.7=88.87%

Beaker No .3
Actual recovery is calculated as above

Theoretical recovery for 1st stage= ((66.67)/ (66.67+50))* 100=X

Theoretical recovery for 2ndstage= (1-X)*((66.67)/ (66.67+50))* 100) =Y

Theoretical recovery for 3Rd Stage= (1-Y) *((66.67)/(66.67+50))*100 )=Z

Total recovery =X +Y+Z


Similarly calculate for beaker no 4 and beaker no 5
Plot the graph for % recoveries vs No. of stages

RESULT
The percentage actual recovery vs no of stages keeping the solvent to feed ratio constant has
been drawn.

INFERENCE

7
COUNTER CURRENT LEACHING
OBJECTIVE

To find the overall stage efficiency of a continuous counter current leaching unit by
batchsimulation of a counter current cascade.

APPARATUS & CHEMICALS

 500 cc beakers (5 nos)


 Burette
 Pipettes(50 cc ,20cc ,5cc)
 Volumetric flask(100 cc,500 cc , 250 cc)
 Conical flask(250 cc) 2 nos
 Filtering funnel
 Sand
 Sodium carbonate
 HCl (approx. 0.1 N)
THEORY

A schematic diagram for 3-stage counter current leaching unit is shown below

In counter current leaching operation the solids to be leached and the solvent move in opposite
directions i.e. the leached solids from the first stage is fed to the second stage as feed, the leached

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solids from the second stage is fed to the third stage as feed etc. while the extract from the nth
stage is used as solvent for the (n-1)th stage, the extract from the (n-1)thstage is used as solvent
for (n-2)ndstage and so on. One usual calculation ,the designer of the leaching unit has to do is to
calculate the no.of stages required to reduce the solute concentration of solid to some specified
value , knowing the amount and solute concentration of leaching solvent. One way to do this
calculation is equilibrium or ideal stage approach. Ideal stage is defined as the stage from which
leaving phases are in equilibrium. But in actual practice , more no.of stages will be required
because of inadequate contact time allowed in each stage, adsorption of solute on the inert solid,
inadequate settling time allowed for solid which may cause carry over of inert solids with the
extract. The ratio of no. of ideal stages to no. of actual stages is called overall stage efficiency.

PROCEDURE

About 50 gm of sodium carbonate is exactly weighed and transferred to a 500 cc volumetric


flask and the volume is made up with distilled water. About 10 gm of sand is exactly weighed
into each one of five different beakers. To each beaker 50 cc of the prepared solution is added.
The beakers are numbered B1, B2, B3, B4& B5. The method of batch simulation of counter
current cascade is as follows. 200 cc of water is added to beaker B1 and after stirring well and
allowing the sand to settle, 200 cc of clear solution is pipetted out and discarded. Now the
contents of this beaker B1 are again extracted with 200 cc of water and 200 cc of extract from
this beaker is transferred to beaker B2 using a pipette. 200 cc of clear solution from this beaker is
discarded. This procedure is continued till all operations as in fig are completed.

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200 cc of extract from B4 is transferred to a clean dry conical flask. The solution is filtered into
another clean dry conical flask. By this stage steady state operation might have attained which
has to be tested. For this, 50 cc of solution extracted from B4 is pipetted into a 250 cc volumetric
flask and the volume is made up with distilled water. 20 cc of this solution is taken in a clean
conical flask and titrated against 0.1 N HCl taken in a burette. Now the leaching process is
continued as in fig. The solution obtained as extract from B5 is filtered, diluted and titrated
against 0.1 N HCl. If the titre value is same as that obtained earlier (for extract from B4), steady
state counter current operation has been attained. If the titre values are different, the procedure is
continued as in figure given below till a steady state titre value is attained for the extract from the
last beaker added to the series. Thus a counter current cascade has been simulated.

If the solution from B4 and B5 concordant titre values, the solution of leached solids from stage
3 is filtered into a clean dry conical flask. 40 cc of this solution is titrated against HCl taken in
burette. If the solution from B5 and B6 concordant titre values, the solution of leached solids
from stage 4 is filtered into a clean dry conical flask. 40 cc of this solution is titrated against HCl
taken in burette. From this titre value , the under flow concentration can be calculated.

A standard solution of Na2CO3 is prepared and this is used to standardize the HCl used in
titrations.

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OBSERVATIONS

Weight of Na2CO3 taken in 500 cc flask =

Weight of sand taken in each beaker =

Volume of solution taken for each feed sample =

Standardisation of HCl

Weight ofNa2CO3 taken in 100 cc volumetric flask =

Volume of Na2CO3 Titre value of HCl (ml)


solution ml
Tit 1 Tit 2 Tit 3

Titre value of HCl

Vol. of Vol.of Vol. of soln.


extract diluted taken for
used for extract titration cm3 Tit 1 Tit 2 Tit 3
dilution cm3

cm3

B4

B5

B3

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CALCULATIONS

Normality of standard Na2CO3 solution =

Normality of HCl =

NHCl ∗ Titre value of HCl ∗ made up vol. of dilute extract


Normality of extract =
Vol. of soln. taken for titration ∗ vol. of extract used
Weight of Na2CO3 in 200 cc of extract = (N extract*53*200)/ 1000

In this calculation , we neglect the change in volume of solution on addition of Na2CO3. In other
words, amount of solvent (A) in each extract phase is to be assumed to be 200gm.

𝑁𝐻𝐶𝑙 ∗ 𝑇𝑖𝑡𝑟𝑒 𝑣𝑎𝑙𝑢𝑒 𝑜𝑓 𝐻𝐶𝑙


𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦 𝑜𝑓 𝑙𝑒𝑎𝑐ℎ𝑒𝑑 𝑠𝑜𝑙𝑖𝑑 𝑠𝑜𝑙𝑛. =
𝑉𝑜𝑙. 𝑜𝑓 𝑙𝑒𝑎𝑐ℎ𝑒𝑑 𝑠𝑜𝑙𝑖𝑑 𝑠𝑜𝑙𝑛. 𝑡𝑎𝑘𝑒𝑛 𝑓𝑜𝑟 𝑡𝑖𝑡𝑟𝑎𝑡𝑖𝑜𝑛

Weight of Na2CO3 in 50 cc of solution adhering to leached solids

= ( Nleached solids *53*50) /1000

x1 = C/(A+C ) = gm of Na2CO3 in 200 cc of extract/ (200+ gm of Na2CO3 in 200cc of extract )

yF= ( gm of Na2CO3 taken in each feed ) / (50+ gm of Na2CO3 taken in each feed )

NF=( gm of sand taken in each feed ) / ( 50+ gm of Na2CO3 taken in each feed )

N3, act = gm of sand taken in each feed / (50+ gm of Na2CO3 taken in leached solids)

y3, act= gm of Na2CO3 in leached solids / (50+ gm of Na2CO3 taken in leached solids)

A rectangular co-ordinate with N on the y-axis and x, y on the x-axis is used for graphical
calculation. We take different y-values and for each one of these calculate N using equation
given below.

C = ( A* y )/(1-y)

N = B / (A + C) =

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Sl. No. 1 2 3 4 5 6 7 8 9 10

C gms

N for
locus of
underflow

Plot equilibrium curve , construct stages and find out No. of theoretical stages.

From graph, y2 =
y3 =
Fractional stage required = (y3,act- y2 )/ (y3 - y2)

Integral no. of stages required =

Overall stage efficiency = ( no. of theoretical stages)/ (no. of actual stages)

RESULT

The overall stage efficiency of a continuous counter current leaching unit by batch simulation of
a counter current cascade has been found to be ________________

INFERENCE

13
ADSORPTION ISOTHERM

OBJECTIVE

To verify the applicability of theFreundlich equation for adsorption of acetic acid on activated
carbon and to determine the value of the constant k and n in the equation c*=k [v (c0-c*)] n

APPARATUS

 Reagent bottles (5nos.)


 Bottle shaker
 Burette
 Filtering funnel (5nos.)
 Conical flask (250cc.5nos.)
 Pipettes (10ml,20ml)
 Volumetric flasks (100ml, 250ml)
 Weighing balance

CHEMICALS

 Acetic acid
 Activated carbon
 Approximately 0.1N NaOH
 Oxalic acid

THEORY

Adsorption operation exploits the ability of certain solids preferentially to concentrate specific
substances from solution to their surfaces. In this components of either liquid or gaseous
solutions may be separated from each other. Some applications of adsorption in gaseous
separations are dehumidification of air and other gases, removal of objectionable odours and
impurities from industrial gases, recovery of valuable solvents vapours from dilute mixtures
with air and other gases and fractionation of mixtures of hydrocarbon gases containing such
substances like methane, ethylene and propylene. Typical liquid separations are removal of
moisture dissolved in gasoline, decolourisation of petroleum products and aqueous sugar
solutions, removal of objectionable taste and odour from water and fractionation of mixture of
aromatic and paraffin hydrocarbons. Adsorption can be physical or chemical. Physical
adsorption or Vander waal’s adsorption can be readily reserved and is the result of
intermolecular forces of attraction between molecules of solid and the substance adsorbed. The

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equilibrium partial pressure of the substance adsorbed equals that of the contacting gas phase.
This is lower than the vapour pressure and so adsorption is not simple condensation. By
lowering the pressure of the gas phase or by raising the temperature, the adsorbed gas is readily
removed or desorbed in unchanged form. Reversible adsorption is seen in liquids as well.
Chemisorption or activated adsorption is the results of chemical interaction between the solid
and the adsorbed substance. The process is frequently reversible, and an adsorption, the original
substance will be found to have undergone a chemical change. Chemisorption finds applications
in catalysis. The usual adsorbants are fuller’s earth, activated carbon, clays, bauxite, alumina,
bone charcoal, decolorizing carbon, gas adsorbent carbon, silica gel, zeolites and metal
aluminosilicates.

Adsorption equilibria

The amount of substances adsorbed depends on the concentration of the contacting gas or liquid
phase, the temperature and pressure. A relationship among these variables is called “adsorption
equilibria”. Data on adsorption equilibria are essential for designing adsorption unit.
Equilibrium data expressed for a particular temperature is called “adsorption isotherm”.

In liquid, adsorption isotherms are important since no appreciable volume changes of the liquid
occur which might be used as a measure of the adsorption. Withdrawal of the solid and weighting
it, as can be done in the case of gases, will not distinguish between the adsorbed liquid and that
which is mechanically included. When adsorbent is mixed with a binary solution, adsorption in
both solute and solvent occurs. Since the total adsorption cannot be measured, the relative or
apparent adsorption can be determined instead. The customary procedure is to treat a known
volume of solution with a known weight of adsorbent, v cm3 of solution /gm of adsorbent.

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As a result of preferential adsorption of solute, the solute concentration of the solution is observed
to fall from the initial value C0 to the final value C* in the liquid. The apparent adsorption of
solute, neglecting any adsorption of solvent is V (C0-C*) grams of solute adsorbed per gram of
adsorbent. This is satisfactory for dilute solutions where the fractions of the original solvent,
which may be adsorbed, is small. Over a small concentration range and particularly for dilute
solutions, the adsorption isotherm may be described by an empirical expression usually attributed
to Freundlich.

C*=k [V (C0-C*)] n

Where k and n are constants at a particular temperature. It is to be noted that n is independent of


units used and k has units same as that used for C*or C0 . Sometimes this curve may show
deviation from linearity. This may be due to appreciable adsorption of the solvent or simply the
general in applicability of the Freundlich expression.

PROCEDURE

Record the room temperature. Weigh about 25gms of acetic acid exactly in weighting tube and
transferred completely by repeated washings to a 250ml volumetric flask (f1).Make up the volume
with distilled water. Pipette out 10ml of this solution in to a 250ml volumetric flask (f2) and the
volume is made up. Weigh about 5gms of activated carbon into a reagent bottle (B1). Add 200ml
of solution from flask (f2) to this bottle. Repeat the same procedure with bottles numbered (B2)
(B3) (B4) (B5) with the difference that the volumes of solution pipette out from the flask(f1) are
20ml,30ml,40ml and 50ml respectively. Shake the bottles well for one hour using the bottle
shaker for adsorption to come equilibrium. Meanwhile, prepare a standard solution of oxalic acid
(approx. 0.1N) and use this to standardize the supplied NaOH solution. Filter the solutions in the
5 bottles. Take NaOH in the burette and titrate it against 10ml of the sample solution.

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OBSERVATIONS

Room temperature =

Weight of acetic acid taken in 250ml flask (f1) =

Preparation of mixtures:-

Bottle no. Vol. taken from Vol. of solution transferred Wt. of carbon taken

f1 to 250cc flask f2 to bottle from f2

Standardization of NaOH:-

Weight of oxalic acid taken =

Volume of solution prepared =

Normality of oxalic acid solution =

Titre value of oxalic acid in ml

Volume of NaOH solution ml Tit .1 Tit .2 Tit.3

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Titration of filtered solution [Filtered solution Vs NaOH-Phenolphthalein]

Bottle no. Volume of filtered solution Titre value of NaOH


taken (ml)
Tit. 1 (ml) Tit. 2 (ml)

CALCULATIONS

Vox ∗ Nox
The normality of given NaOH solution =
V NaOH

The value of v (cm3 of solution / g of adsorbent) and co in each of the five bottles are
calculated.

cm 3 ofsolution
V =
g of adsorbent

wt .of CH 3 COOH ∗ vol .of CH 3 COOH


Co =
250 ∗ 250

The value of c* in each of the original filtered solution is found by

N NaOH ∗volume of NaOH Eq .wt .of acetic acid


C*= *
Volume of filtered acetic acid soln . 1000

log [ V (Co – C*)] =

log C* =

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Bottle no. V(cm3soln./ Co (solute / C* (gm of Co –C* Log [V(Co –C*)] log C*
gm cm3 solution) solute/cm3soln)
adsorbent)

From graph, slope n =

y-intercept, log k =

RESULT

From the graph, between log C * and log [V (Co - C*)], the value of k and n was
determined.

k= n=____________

INFERENCE

19
BATCH DRYING
AIM

To plot moisture content vs time graph and then the rate of drying vs moisture content curve for a
given feed.

APPARATUS REQUIRED

Crucible, weighing balance, measuring cylinder etc

CHEMICALS REQUIRED

Calcium carbonate

THEORY

The moisture contained in a wet solid or liquid solution exerts a vapor pressure to anextent
depending upon the nature of the moisture, the nature of the solid and thetemperature. If a wet solid
is exposed to a continuous supply of fresh gas containing afixed partial pressure of the vapour, the
solid will either lose moisture by evaporation orgain moisture from the gas until the vapor pressure
of the moisture of the solid equalspartial pressure of the vapour in air stream. Thereafter, the mixture
to be dried retains theequilibrium content for the prevailing conditions.

Rate of drying rate curve has two major parts, a period of constant rate and one of falling rate. If a
solid is initially very wet, the surface will be covered with a thin film of liquid, which is entirely
unbound moisture. When it is exposed to relatively dry air, evaporation will take place from the
surface.

When the average moisture content of the solid has reached the critical moisture content, the surface
film of moisture has been so reduced by evaporation that further drying causes dry spots to appear
upon the surface; these spots occupy increasingly larger proportions of the exposed surface as drying
proceeds. Since however, the drying rate is computed by means of the constant gross surface, the
drying rate must fall even though the rate per unit of wet surface remains constant. This give rise to
the falling rate period called unsaturated surface drying.

Rate of drying ,N=(-Ss/A)dX/dt.

Ss is the weight of dry solid; A is surface area of solid exposed to air.

dX/dt is the slope of the curve , moisture content ( X) vs time (t)

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PROCEDURE

Take 9 crucibles and mark them as 1, 2 ... 9. Take about 10 gm of calcium carbonate in all nine
clean & dried crucibles. Add about 9 ml of water into all the crucibles. Mix it thoroughly &
uniformly using a glass rod and place it in a dryer working at 65°C. At t=1 min, take out the crucible
marked 1, cool it for a minute and weigh. Calculate the moisture that is lost to the air by
vaporization. At t=3 min, take the crucible marked as 2, and repeat the procedure. Take the rest of the
crucibles at t= 5,10,15, 30, 60, 90 & 120 min. Plot kg of moisture content/kg of dry solid (X) Vs time
(t). Find out slope (dX/dt) of this curve at different points and calculate the rate of drying using the
formula N= (-Ss/A)*dX/dt.

Here Ss is the weight of dry solid; A is surface area of solid exposed to air.

Plot the N Vs X graph

OBSERVATIONS

Weight of crucible =

Amount of water poured =

Weight of crucible + sample (before drying) , B=

Weight of sample+ crucible (after drying), C =

Weight of dry sample Ss=

Area of the sample exposed to the air A=

Time SI. No. of Weight of Weight of Weight of Moisture content


crucible the sample crucible+sample crucibles+ sample of the sample, (kg
(g) before drying B after drying C (g) of moisture/ kg of
(g) dry solid)

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SI no Moisture content Slope dX/dt Rate drying, N = ( -Ss/A)dX/dt

CALCULATION

Moisture Evaporated = B- C
Moisture content = (Initial Moisture content- Moisture Evaporated)/ Wt. of dry sample
Rate of Drying (N) = ( -Ss/A)dX/dt.

RESULT
Moisture content Vs time graph and rate of drying curve for given feed is plotted

INFERENCE

22
SIMPLE-DISTILLATION
AIM

To verify Rayleigh's equation for simple distillation of methanol-water mixture and verify the
material balance equation for methanol.

APPARATUS &CHEMICALS REQUIRED

Simple distillation apparatus, density bottle, measuring cylinder, burette, conical flask, 50 mole %
methanol - water mixture,pure methanol etc.

PRINCIPLE

Distillation is a method of separating the components of a solution. In distillation, the feed


solution is heated so that a part of it vaporizes. The vapors are condensed and collected which is
called the distillate (D). The liquid that is left behind in the distillation still is called the residue
(B). The feed solution is split into two fractions such as the distillate and the residue and the
process is then called binary distillation or binary fractionation. Both distillate and residue shall
contain all constituents of feed, though the distillate will be rich in more volatile constituents
and the residue will be rich in less volatile constituents.

Flash vaporization or equilibrium distillation is a single stage operation where in a liquid


mixture is partially vaporized, the vapor is allowed to come to equilibrium with the residual
liquid, and the resulting vapor and liquid phases are separated and removed from the apparatus.
It may be batch wise or continuous.

Simple or differential distillation consists of infinite no of successive flash vaporization


of a liquid only an infinitesimal portion of the liquid were flashed each time. It is a batch
operation.

For a binary mixture of A and B, assume that at any time during the course of distillation
there are L moles of liquid in the still with a composition x mole fraction and the vapor formed
having mol fraction y* in equilibrium with that of liquid.On vaporizing a small amount of liquid
dL, the composition of liquid changes from x to (x-dx) and the amount of liquid in still becomes
(L-dL).

Material balance for A(the more volatile component)

𝐿𝑥 = 𝑦 ∗ 𝑑𝐿 + (𝐿 − 𝑑𝐿)(𝑥 − 𝑑𝑥)

𝐿𝑥 = 𝑦 ∗ 𝑑𝐿 + 𝐿𝑥 − 𝐿𝑑𝑥 − 𝑥𝑑𝐿 + 𝑑𝑥𝑑𝐿

23
dxdL can be neglected and on rearranging and integrating
𝑥𝐹
𝐹 𝑑𝑥
𝑙𝑛 =
𝑊 𝑦∗ − 𝑥
𝑥𝑊

Where F and W are the total no. of moles of feed liquid and residue at any instant during
distillation having composition xf and xwrespectively. The above equation is known as Rayleigh
eqn.

If xf is the mole fraction of component a in feed, yD that in vapour and xW that in the residual
liquid then a simple material balance equation for component A is written as

Fxf = DyD + WxW

PROCEDURE

About 400 ml of given methanol-water mixture is taken in the simple distillation flask
after exactly determining the specific gravity using specific gravity bottle. The distillation
apparatus is assembled. Circulation of water through condenser is started and heating element is
switched on. Water is taken in one burette and methanol is taken in the other one. A 150 cc
conical flask is cleaned and dried. A 10% by volume mixture of methanol and water is made in
this by mixing 2 ml methanol with 18 ml of water and the specific gravity of this mixture is
found. Similarly specific gravity of several known compositions of CH3OH and H2O is found. It
is better to find the specific gravities for mixtures with increasing percentages of CH3OH and dry
the bottle between successive specific gravity determinations so that the little amount of solution
remaining in the bottle will not affect the experiment. When about 200 cc of distillate has been
collected, heating is stopped and the apparatus is disassembled. The volumes of distillate
collected and that of residue remaining are measured using the measuring cylinder. The specific
gravity of these solutions is also determined.

A calibration curve is prepared with mol % methanol on x axis and specific gravity on y
axis. The composition of feed mixture, distillate and residue are determined using this chart.

To find specific gravity,

Fill the specific gravity bottle with pure water to the brim and close the lid and find the weight
(Wwater). Then, fill the specific gravity bottle with the water-methanol solution to the brim and
close the lid and find the weight (Wsolution). Find Wsolution/Wwater, which gives the specific gravity.

24
OBSERVATION

Determination of composition by specific gravity measurement

Volume of specific gravity bottle =

Volume of CH3OH and H2O mixture taken for distillation (feed)=

Weight of specific gravity bottle =

Weight of specific gravity bottle with solution for distillation (feed) =

Specific gravity of feed =

Volume of distillate collected =

Specific gravity of distillate =

Volume of residue remaining the still =

Weight of distillate with density bottle =

Weight of residue with density bottle =

Specific gravity of residue =

Mixture VolumeOfCH3OH Volume Weight of Weight of sp. Sp. Gr Mol%


ofH2O sp.gravity gravity bottle of CH3OH
No. bottle alone + mixture mixture

1
2
3
4
5
6
7
8
9
10

25
To find mol% of methanol,

Volume of methanol= cc

Volume of water= __________ cc

Mass of methanol = sp gravity of pure methanol * volume of methanol =

Mass of water = sp gravity of pure water * volume of water =

Moles of methanol = mass of methanol/molecular weight of methanol =

Moles of water = mass of water/molecular weight of water =

Mole fraction of methanol =

The equilibrium relationship for CH3OH and H2O system at 1 atm is given in this
following table.

x y*
0 0
0.02 0.134
0.04 0.23
0.06 0.304
0.08 0.365
0.1 0.418
0.15 0.517
0.2 0.579
0.3 0.665
0.4 0.729
0.5 0.779
0.6 0.825
0.7 0.87
0.8 0.915
0.9 0.958
0.95 0.979
1 1

26
The values of l/(y* -x) for different x values are calculated and a curve with x on the x axis and
l/(y*-x) on the y axis is plotted. The area under this curve between xw and xf gives the value
𝑥𝑓 𝑑𝑥
of
𝑥𝑤 𝑦 ∗ −𝑥

CALCULATION

Molecular weight of CH3OH=

Molecular weight of H2O =

Specific gravity of CH3OH =

Mol % of methanol in distillate, yD.av=

Mol % of methanol in feed, xf=

Mol% of methanol in residue xw =

The number of moles in feed, distillate and residue are determined from their mole fractions

For feed F,

Mass fraction of CH3OH in F = xf*MWmethanol/[xf*MWmethanol+(1-xf)*MWwxer]

Mass of F = volume of F * specific gravity of F=

Moles of CH3OH in F=mass of F * mass fraction of CH3OH in F/ MWmethanol=

Similarly calculate moles of water in feed.

Moles of Feed, F = moles of methanol in Feed + moles of water in Feed =

For Distillate D

Mass fraction of methanol in distillate = yDa,*MWmethanol/ [yDav*MWmethanol+(1-yDavg )*MWwater ] =

Mass fraction of water in distillate=

Mass of distillate =volume of distillate *sp.gravity of distillate =

Moles of methanol in distillate =

Moles of water in distillate =

Moles of distillate, D=

27
Residue, W

Mass fraction of methanol in residue = xw*MWmethanol/[xw*MWmethanol +(l-xw)MWwaterJ] =

Mass fraction of water in residue =

Mass of residue = volume of residue * specific gravity of residue =

Moles of methanol in residue =

Moles of water in residue =.

Moles of residue, W =

𝑥𝑓 𝑑𝑥
From graph, = In F/W = ________
𝑥𝑤 𝑦 ∗ −𝑥

Verify the material balance equation Fxf = DyD + WxW

RESULT

Rayleigh’s Equation and material balance equation for simple distillation of methanol water
system was verified.

INFERENCE

28
LIQUID-LIQUID DIFFUSION
Aim:
To determine the diffusion coefficient of a liquid.

Utilities Required:

Electricity Supply: Single Phase, 220 V AC, 50 Hz, 5-15 Amp combined socket with earth
connection. Earth voltage should be less than 5 Volts.

 Water Supply (Initial fill).


 Floor Drain Required.
 Floor Area Required : 1.5 m x 0.75 m
 Weighing balance : least count 0.1 gm
 Chemicals:
NaCl : 100 gms
Distilled water : 5 Lit.
Theory:
Introduction:
Diffusion is concerned with the movement of individual molecules through a substance by virtue
of their thermal energy. The phenomenon of molecular diffusion ultimately leads to a completely
uniform concentration of substances throughout a solution which may initially have been non
uniform.

So this equipment is very helpful in determining the diffusion coefficient of liquid. We can also
study the effect of temperature on diffusion coefficient

When two solutions of different concentration, originally at equilibrium with their surroundings,
are contacted, a concentration gradient is created and mass transfer starts until a new equilibrium,
In case of no motion or convection species moves through interface by diffusion from high to
low concentration regions.

Increase in concentration of bulk liquid is a result of diffusion, and can be determined as a


function of time by an indirect measurement of ionic conductivity. Fick's law together with a
proper relation between concentration and conductivity can be used to determine the diffusion
coefficient of salt in water.

Description:
The equipment consists of a tube made of glass, placed in a vessel. Water bath is provided with
heater. Temperature of the vessel is controlled by PID controller. Stirrer is provided to maintain
the constant temperature in bath. A conductivity sensor with indicator is provided to observe the

29
change of conductivity of water in vessel. Drain valves are provided to drain the water from bath and
reactor vessel.

Procedure:
StartingProcedure:
 Prepare 1L 1M NaCl solution by dissolving 58.4 gm of sodium chloride in 1L
of distilled water.
 Clean the apparatus and make it free from dust.
 Close all the valves V1 to V2.
 Ensure that switches given on the panel are at OFF position.
 Fill the bath with water 3/4thof its capacity.
 Fill Known amount of distilled water inside the vessel.
 Switch ON the main power supply.
 Set the temperature of water in vessel by increasing or decreasing button
through PID controller.
 Switch ON the heater and switch ON the stirrer for bath & vessel.
 Wait till the temperature of water inside the vessel attains the set value (SV).
 Fill the Glass tube with NaCl solution and kept in the vessel in such a way that the tube
membrane is just dip the level of water in vessel (say 4mm).
 Start the stopwatch and record the change of conductivity of water with respect to time.
 Repeat the experiment for different temperatures.
 Repeat the experiment for different molarities of NaCl solution.
Closing Procedure:

 When experiment is over, Switch OFF heater and stirrer.


 Switch OFF the main power supply.
 Remove the tube from vessel & Clean the tube and drain the water from bath by
opening the drain valve V2 and vessel by opening the drain valve V1.

30
Observation & Calculation:

Data:
Molecular weight of salt, Wm = 58.4 g/mole
Diameter of membrane, d = 1.6 cm

Observation Table:
Weight of salt, W = .............. g
Volume of water containing salt, Vw = .............. ml
Volume of water in vessel, V = ..............Ltr

S.No. t (min) K (mS)

Calculation:

 d
2

a (cm2)
4

W  1000
M  (m)
Wm  Vw

 W 
   1569.8  0.8
Cm   Vw 
(Ω-1. L.mol-1)
1000 M

Plot the graph K vs. t & Calculate slope dK/dt.

V  dK/dt
D (cm2/s)
a  M  Cm

31
M Cm D
S.No.
(m) (Ω . L.mol-1)
-1
(cm2/s)

RESULT

The diffusion coefficient of the given liquid has been determined

INFERENCE

32
VAPOUR IN AIR DIFFUSION

Aim:
To determine the diffusion coefficient of an organic vapor (i.e. CCl4) in air.
Utilities Required:
 Electricity Supply: Single Phase, 220 V AC, 50 Hz, 5-15 Amp combined socket
with earth connection.
 Water Supply (Initial fill)
 Floor Drain Required.
 Floor Area Required: 1.5 m x 0.75 m
 Chemicals:
 CCl4 : 200 ml
 Water : 10 Ltrs

Theory:
Diffusion is concerned with the movement of individual molecules through a substance by virtue
of their thermal energy. The phenomenon of molecular diffusion ultimately leads to a completely
uniform concentration of substances throughout a solution which may initially have been non
uniform. So this equipment is very helpful in determining the diffusion coefficient of an organic
vapour. We can also study the effect of temperature on diffusion coefficient.
If two gases are inter-diffusing with continual supply of fresh gas and removal of the products of
diffusion, this diffusion reaches an equilibrium state with constant concentration gradients. This is
known as steady state diffusion. If also there is no total flow in either direction the rates of diffusion
of A and B, NA and NB are equal but have opposite sign.
According to Dalton’s law the total concentration of the two components CA and CB is Constant

Then using the integrated form of the Fick Diffusion equation with appropriate

Where PA1 and PA2 are the partial pressures of A at the boundaries of the zone of diffusion and x is
the distance over which diffusion occurs.

In case where gas A is diffusing through stagnant gas, B (non-diffusing) the flow carries both
components in proportions to their partial pressure

The total transfer of A is the sum of this proportion of the flow and the transfer by diffusion

33
And

This is the expression used for the experimental determination of vapour diffusion coefficients in
gases by evaporation from a liquid surface in a narrow bore tube and measuring the fall of level of
this surface. The distance of the liquid surface below the open end of the tube is measured before and
after evaporation over a definite period. If the variation in level is small then arithmetic mean of
these two readings is taken as the value of x. In case there is appreciable change of level, the value of
x is determined by integration between the initial and final readings of level.
The rate of evaporation is thus given by:

Integration of this expression yields:

34
Other form of this equation that is convenient to use is:

Where DAB diffusivity coefficient P, PBM and R are total pressure log mean pressure and real gas
constant. To is operating temperature, MA is molecular weight of component A. t is time taken in
diffusion process
Procedure:
Starting Procedure:
 Clean the apparatus and make it free from dust.
 Ensure that switches given on the panel are at OFF position.
 Fill the water bath with water 3/4th of its capacity.
 Set the water bath temperature (approx 50oC).
 Switch ON the main power supply.
 Switch ON the heater.
 Switch ON the stirrer.
 Wait till the bath attains the set temperature. Note the steady temperature
of the bath.
 Fill the T-tube with CCl4 solution up to two centimeters of the capillary leg.
 Note down the initial height of liquid in the capillary.
 Make the connection with air pump and allow a gentle current of air to flow
over the capillary.
 Record the height of liquid in the capillary after every 30 min. .
 Repeat the experiment for different water bath temperatures.
 Repeat the experiment for different organic liquids like: ethanol, toluene,
acetone and hexane.
Closing Procedure:
 When experiment is over stop the air supply.
 Switch OFF heater and stirrer.
 Switch OFF the main power supply.
 Clean the tube and drain the water bath by open the valve V1.
Observation & Calculation:
Data:
Total pressure P = 1.01325x105 N/m2
Real gas constant R = 8.314 (N/m2)-m3 /mole-K
Molecular weight of the liquid MA = 154 g/mole
Partial pressure of liquid at the top of the tube PA2 = 0 N/m2
Constant A = 15.84
Constant B = 2790.78
Constant C = 226.46

35
Observations:
T = ________ oC
Xo =________ cm
Observation Table:
Sl.No. t ( min) X (cm )

Calculations:

( CCl4)=_________ (kg/m3)

X = (Xo / 100) m [Initial height of liquid at t1 = 0]

x = ( X/100) m

t1 = t x 60 s
Calculation table

Sl.No. t 1 ( s) x(cm)

36
Nomenclature:

Precaution & Maintenance Instructions:


 Carbon tetrachloride (CCl4) should be colorless.
 Don’t switch ON the heater before filling water in the bath.
 Microscope focus should be clear, if not then adjust it.
Troubleshooting:
 If the temperature is not increasing after switch ON the heater, check the
continuity of heater.
 If the DTC displays 1 on the screen it means the computer socket is not
connected so connect it.
 If the meniscus is not clear adjusted focus the lens.
 If the movement of the microscope is not smooth put some lubricating oil on it.

37
RESULT

The diffusion coefficient of the given organic vapour in has been determined

INFERENCE

38
STEAM DISTILLATION

AIM:
To determine vaporization and thermal efficiencies for steam distillation of turpentine

APPARATUS
 The steam distillation apparatus
 Specific gravity bottle
 Measuring cylinder
 Separating funnel
PRINCIPLE
At atmospheric pressure high-boiling liquids cannot be purified by distillation since the
components of the liquid decompose at the high temperatures required. In steam distillation the
temperature of liquid is reduced by vapourizing the material into to a stream of carrier vapour,
the liquid phase which is immiscible with the material being distilled. By mixing material to be
distilled with an immiscible liquid, the mixture can be made to vapourize at a temperature much
lower than its normal boiling point. A mixed vapour of carrier and vapourized material is taken
overhead and condensed, and liquid layers each containing one of the components, are separated
by gravity. Since steam is readily available, it is widely used as immiscible carrier vapour in
many distillations. Steam distillation is used to separate high-boiling component from small
amount of non-volatile impurities. Steam distillation is used in food industry for removal of
volatile impurities and flavors from edible fats and oils.

In steam distillation a high-boiling liquid (A) is distilled along with steam (B), which is
immiscible with A .When the two components A and B which are immiscible exert their own
vapor pressure and when the sum equals total pressure of the system the mixture begins to boil.
By steam distillation as long as liquid water is present component A vaporizes at a temperature
well below its normal boiling point without using a vacuum. The vapors of high-boiling liquid
and water are condensed and the two immiscible phases should be separated. The mole fraction
of either of the components in the vapor phase will be proportional to its vapor pressure.
Therefore, theoretical or minimum amount of water distilled along with the given immiscible
liquid (A) can be calculated from the relationship,

(WA/WB)min = (MA PA) / (MB PB)

Where WA& WB are weights of component turpentine and water in vapor phase, Kg
PA& PB vapor pressures of component turpentine and water at distillation temp., atm
MA& MB molecular weights of turpentine and water
In actual practice, when liquid water is present,

(WA/WB) act = [MA (P-ƞsPB)] / (MB ƞs PB) = (MA PA)/ (MB ƞs PB)

ƞs = vapourization efficiency

39
vapourization efficiency = ƞs = [ (WA/WB)min] / [(WA/WB) act]
Thermal Efficiency = ( Minimum steam requirement for distillation per unit weight
turpentine distilled) / ( Actual steam requirement for distillation per
unit weight turpentine distilled )

Actual steam requirement for distillation per unit weight turpentine distilled = [W A,act+ Wt. of
water in still- (steam used in heating the residual turpentine to boiling temp] / W B,act

Minimum steam requirement for distillation per unit wt. of turpentine distilled=
(WA/WB)min + [0.5 (t-troom) +71.1] / [ 0.45(100- t)+539 ]
wheret is the temp of distillation

PROCEDURE:

1) Fill the boiler with water till the drain cock level.

2) Switch on the steam boiler

3) Find the specific gravity of impure turpentine and take 300ml of that in the still

4) Connect the condenser to the still and allow water to flow through the condenser

5) Open slightly the steam outlet valve on the boiler. Ensure that not much of steam comes out of
the condenser.

6) Maintain constant pressure of the steam throughout the experiment.

7) When the temperature inside the flask starts rising up and at a particular temperature it
remains constant, note down this value of as boiling point of mixture .

8) Collect the condensate in a conical flask. Continue the distillation to get around 200ml
distillate.

9) Separate the two phases of both residue and distillate using a separating funnel and note down
volume of each phase.

10) Measure the specific gravity of pure turpentine

..OBSERVATION AND CALCULATION:

Room temperature tR = _________ 0C


Sp. gravity of water at tRρW = _______________
Weight of sp. gravity bottle W1 = __________________ gm
Weight of sp. gravity bottle + water in distillate W2 = ______________ gm
Weight of sp. gravity bottle + turpentine in distillate W3 = ____________ gm
40
Sp. Gravity of turpentine in distillate, ρOD = [(W3 – W1) / (W2 – W1)] * ρW = ____gm/cc
Weight of sp. gravity bottle + turpentine in residue W4 = ____________ gm
Sp. Gravity of organic liquid in residue, ρOR = [(W4 – W1) / (W2 – W1)] * ρW = ____gm/cc

Volume of turpentine in distillate VOD = ______________ cc


Mass of turpentine in distillate, MA = VOD * ρOD = ____________ gm
Volume of aqueous lager in distillate, VWD = _______________cc
Mass of aqueous layer in distillate, MB= VWD * ρW = ____________ gm
Actual mass ratio (WA / WB)= _____________
(WA/WB)min = (MA PA) / (MB PB)

PA =vapour pressure of turpentine at distillation temperature


PB = vapour pressure of water at distillation temperature
Hausbrand’s Chart[Data from Perry (VI Edition; Pg 3-59 ; T 3-8)]

Vapour Vapour Vapour


Pressure of Vapour Pressure of Pressure
Temperature turpentine Pressure of Temperature turpentine of water
0 0
C atm water atm C atm atm
60 0.0346 0.1964 87.7 0.1081 0.635
65.5 0.0442 0.2528 93.5 0.1339 0.7837
71 0.055 0.3223 99 0.1645 0.9603
76.5 0.0686 0.4074 104.5 0.2012 1.1686
82 0.087 0.5106 110 0.2475 1.413

41
Theoretical or minimum mass ratio is = (WA / WB)min

At point P, PA = PT - PB

PB = PT - PA

Vaporization efficiency is = [(WA / WB)min/ (WA / WB)act ] * 100 = ____________%

Volume of organic layer in residue, VOR = ________________ cc

Volume of aqueous layer in residue, VAR = ________________ cc

Mass of organic layer in residue, = VOR * ρOR = ___________ gm

Mass of aqueous layer in residue, = VAR * ρW = ___________ gm

Latent heat of vapourization of Turpentine T = 71.1 cal/gm

We assume that the steam is used saturated steam at 1atm

Latent heat of vapourization of steam at 1 atm, s = 539 cal/gm

Specific heat of turpentine = 50 cal/ gm 0C

Specific heat of steam = 0.45 cal/ gm 0C

Actual steam requirement for distillation per unit weight turpentine distilled = [W A,act+ Wt. of
water in still- (steam used in heating the residual turpentine to boiling temp] / W B,act

Minimum steam requirement for distillation per unit wt. of turpentine distilled=
(WA/WB)min + [0.5 (t-troom) +71.1] / [ 0.45(100- t)+539 ]

42
where t is the temp of distillation

Thermal Efficiency = ( Minimum steam requirement for distillation per unit weight
turpentine distilled) / ( Actual steam requirement for distillation per
unit weight turpentine distilled )

RESULT

Thermal Efficiency=__________________

Vapourization Efficiency=__________________

INFERENCE

43
CROSS CURRENT LEACHING
OBJECTIVE

To find the overall stage efficiency of a continuous cross current leaching operation by
batch simulation of a cross current cascade.

APPARATUS & CHEMICALS

 500 cc beakers (5 nos)


 Burette
 Pipettes
 Volumetric flasks
 Filtering funnel
 Sand
 Sodium carbonate
 HCl (approx. 0.1 N)
THEORY

In a continuous leaching operation, it is either done in a battery of contacting units or stages. In a


cross current system the solids from each stage is contacted with fresh solvent

Notation Schemes Used


A-Solvent B-Inert solid C-Solute
We do the calculations on an inert free basis as explained below

44
Graphical representations can be made on a rectangular coordinate system by taking N on the Y-
axis and x or y on the X-axis.

Material balance of solute in any stage is


……………… (1)
Material balance on solution (A+C) is
……………… (2)
Material balance on inert solids is
………………. (3)
From equations (1), (2) and (3)

….…………….. (4)

Equation (4) will be a straight line passing through the points E, M and R.

An ideal stage is one in which the resultant solution leaving the stage is of the same composition
as the solution adhering to the solid leaving the stage. In actual practice more stages will be
required. The ratio of the number of ideal stages to the number actual stages required to
accomplish the same results is called the overall stage efficiency.

PROCEDURE

A standard solution of Na2CO3 is prepared and this is used to standardize the HCl used in
titrations.

About 5 gm of sodium carbonate is exactly weighed and transferred to a 500 cc beaker. About 45
gm of sand is exactly weighed and added to the beaker. Add 50 cc of water. The contents in the
beaker act as the feed. The method of batch simulation is as follows. 200 cc of water is added to
beaker and after stirring well and allowing the sand to settle, 200 cc of clear solution is pipetted
out and the extract is discarded. Now the contents of the beaker is again extracted two more
times with 200 cc of water and 200 cc of extract from this beaker is pipetted out and extract is
discarded. Thus a cross current cascade has been simulated for a 3 stage operation. About 20 ml
of the underflow solution of the last stage is taken and titrated against standardised HCl and the
concentration of solute in the underflow is found out.

45
OBSERVATIONS

Weight of Na2CO3 taken in 500 cc beaker =

Weight of sand taken in 500 cc beaker =

Volume of water taken in feed sample =

Volume of Solvetn added in each stage =

Titre Value when leached solid solution is titrated

against HCl =

Standardisation of HCl

Weight ofNa2CO3 taken in 100 cc volumetric flask =

Normality of standard Na2CO3 solution

Volume of Na2CO3 Titre value of


solution ml HCl , ml

A rectangular co-ordinate with N on the y-axis and x, y on the x-axis is used for graphical
calculation. We take different y-values and for each one of these calculate N using equation
given below.
C = A*y / (1-y)

N = B / (A + C)

Sl. No. 1 2 3 4 5 6 7 8 9 10

C gms

N for
locus of
underflow

46
CALCULATIONS

Normality of standard Na2CO3 solution =

Normality of HCl =
NHCl ∗Titre value of HCl
Normality of leached solid solution = Vol .of leached solid solution taken for titration

Weight of Na2CO3 in 50 cc of solution adhering to leached solids


Normality of leached solids solution ∗53∗50
= 1000

Stage 1 Overall Material Balance

F + RO1 = E1 + R1 = M1

Solute Balance

FYF + RO1X0 = E1Y1 + R1X1 = M1Ym1

X0 = 0

𝐹𝑌𝐹
∴ 𝑌𝑚1 =
𝐹 + 𝑅𝑚1

From Graph N1= __________

Y1 = _____________

Stage 2 Overall Material Balance

E1 + RO2 = E2 + R2 = M2

Solute Balance

E1Y1 + RO2X0 = E2Y2 + R2X2 = M2Ym2

X0 = 0

𝐸1 𝑌1
∴ 𝑌𝑚2 =
𝐸1 + 𝑅𝑂2

From Graph N2= __________

Y2 = _____________

𝐸2 𝑌2
𝑌𝑚3 =
𝐸2 + 𝑅𝑂3

47
y1=_______________

y3(actual)=C/(A+C)

Actual no. of stages=3

From graph,

y2 = & y3 =___________

Fractional stage required = (y3,act- y2 )/ (y3 - y2)

Integral no. of stages required =____________

Overall stage efficiency = ( No. of theoretical stages)/ (No. of actual stages) =__________

RESULT

The overall stage efficiency for cross current leaching cascade has been found to be__________

INFERENCE

48
ABSORPTION IN PACKED BED
OBJECTIVE:

To study the absorption of carbon dioxide by aqueous sodium hydroxide solution in a packed
bed absorption tower.

AIM:

1. To calculate the overall mass transfer coefficient (KGa).


2. To calculate the number of transfer units (NTU).
3. To calculate the height of transfer units (HTU).
INTRODUCTION:

In absorption a gas mixture is contacted with a liquid for preferential dissolution of one or more
components of the gas in liquid. Such operation requires transfer of mass from gas stream to the
liquid. In many industrial applications, the absorption process is accompanied by chemical
reaction usually; reaction in the liquid of the absorbed component with a reagent in the absorbing
liquid takes place. The reagent and the product of reaction may be soluble e.g. absorption of CO2
into an aqueous solution of ethanol amines or other alkaline solutions. Reaction of the absorbed
solute provides higher absorption rates due to:

 Destruction of the absorbed solute as it forms a compound reduces the equilibrium partial
pressure of the solute that in turn increases the concentration difference between the bulk
phase and the interface.
 Increase in liquid phase mass transfer coefficient.
THEORY:

Packed towers, used for continuous contact of liquid and gas in both counter current and co
current flow, flow are vertical columns which have been filled with packing or devices of large
surface. The liquid is distributed over, and trickles down through, the packed bed exposing a
large surface to contact the gas. Many industrial absorption processes are accompanied by
chemical reaction. Reaction in the liquid of the absorbed component with a reagent in the
absorbing liquid is especially common.

49
50
DESCRIPTION

UTILITIES REQUIRED:

51
EXPERIMENTAL PROCEDURE:
STARTING PROCEDURE:
1. Prepare 2 N NaOH feed solution by dissolving 800 gm NaOH pellets in 10 liter of
distilled water.
2. Fill one burette by 1N HCl solution.
3. Take 25 ml BaCl2 in a conical flask.
4. Close all the valves V1-V8.
5. Fill the prepared solution in feed tank by open the valve V4 and air vent valve V5.
6. Close the valve V4-V5.
7. Connect compressed air supply by open the valve V6.
8. Connect electric supply to the set-up.
9. Start the supply and fix the flow rate of NaOH solution by adjust the valve V1.
10. Note down the flow rate of NaOH solution.
11. Wait till the overflow, now start the supply of CO2 and compressed air.
12. Fix the flow rate of CO2 by open the valve V3 and compressed air by adjust the valve V2
(CO2 should be in the range of 3.33-16.67%).
13. Note down the flow rate of CO2 and compressed air.
14. Wait for 10 minute, collect 10 ml sample in conical flask that already contains 25 ml of
BaCl2.
15. Titrate the sample solution against 1N HCl using phenolphthalein as an indicator (add
HCl from burette).
16. Repeat the experiment for different flow rates of CO2 and compressed air.
17. Repeat the experiment for different flow rates of NaOH solution.
CLOSING PROCEDURE:
1. When experiment is over stop the supply of CO2 and compressed air.
2. Switch OFF the main power supply.
3. Drain the feed tank by open the valve V7.
4. Drain the column by open the valve V8.

52
OBSERVATION & CALCULATION:

53
54
10. PRECAUTION & MAINTENANCE INSTRUCTIONS:
1. Always use distilled water for making feed solution.
2. Clean the packed column by just passing the clean water into the column after conducting
the experiment.
3. Drain the column and feed tank of NaOH after completion of experiment.
4. Close the CO2 cylinder after use.
11. TROUBLESHOOTING:
1. If any types of suspended particles are come in the rotameter, remove the rotameter clean
the tube and fit it at its place.
2. If there is any leakage tight that part or fix it again after wrapping Teflon tape.
3. If rotameter is fluctuating more than average tight the control knob properly.

55
RESULTS

1. The overall mass transfer coefficient (KGa)=_____________


2. The number of transfer units (NTU)=______________
3. The height of transfer units (HTU)=_______________

INFERENCE

56
PACKED BED DISTILLATION COLUMN
AIM
1. To operate the column under total reflux condition and calculate the minimum number of
theoretical stages using Fenske’s equation.
2. To operate the column under any desired reflux condition and calculate theoretical
number of stages using Mc-Cabe Thiele’s method.
3. To calculate the HETP for known packed height.
THEORY
Packed column are often used for distillation when the separation is relatively easy and the
required column diameter is not very large. The column height is generally based on the number
of theoretical plates and the height equivalent to theoretical plate (HETP).

Z=Ntx HETP

Where Z and Nt are packed height and number of theoretical plates respectively.
The operation of a column can be analyzed using the operating line equation as for the rectifying
section of the continuous distillation:

Since the slope of the operating line is R / (R+1), the slope increases as the reflux increases, until
when reflux is infinite. Under total reflux slope is 1. The operating line then coincides with the
diagonal. The number of plate is minimum at total reflux.

Minimum number of plates required can be calculated from the terminal concentration of x B and
xD based on the relative volatility of the components α, which is defined in terms of equilibrium
concentrations:
Minimum number of theoretical plates required is calculated by Fenske’s equation

For the determination of number of theoretical plates at desired reflux ratio the graphical method
which is called McCabe-Thiele’s method is used assuming constant molar flow rate and
neglecting heat effects.

UTILITIES REQUIRED:

1. Electricity Supply: Single Phase, 220 V AC, 50 Hz, 32 Amp MCB with earth
connections.
2. Water Supply: Continuous @ 2 LPM at 1 bar.
3. Chemicals: Water(15 L) and Methanol(4 L)

57
EXPERIMENTAL PROCEDURE

STARTING PROCEDURE:

1. Prepare methanol water solution by mixing known amount of water and methanol. The
composition of methanol in solution should be in the range of 15 to 25 % by volume.
2. The total amount of solution should not be less than 15 liters.
3. Note down the volume of water and methanol.
4. Close all the valves V1-V16.
5. Ensure that switches given on the panel are at OFF position.
6. Fill water in the cold water tank.
7. Fill the reboiler with methanol-water solution by open the valve V1 and air vent valve
V2.
8. Close the funnel valve V1 and the air vent valve V2.
9. Connect electric supply to the set-up.
10. Set a process temperature for the process using the digital temperature controller (DTC).
The temperature should be in the range of 85 to 95 ºC.
11. Start the heater & cooling water pump.
12. Adjust the cold water flow rate by valve V3 to a moderate value.
13. Set the cyclic timer for total reflux.
14. Wait 25-30 minute for the system to achieve steady state.
15. Take out the samples from the bottom & distillate stream (by closing the timer for short
while).
16. Measure the composition of distillate and residue.

CLOSING PROCEDURE:
1. When experiment is over stop the water supply.
2. Switch OFF the pump and heater.
3. Switch OFF the main power supply.
4. Drain the column, reflux drum, receiving tank and water tank.
5. Drain the vessel after temperatures fall down to atmospheric values space by open the
valve V6.

PRECAUTION & MAINTENANCE INSTRUCTIONS

1. Heater should not be switch ON before filling the feed into reboiler.
2. Always drain, tanks and reboiler, when experiment is over.
3. Always use clean water and ensure that there are no foreign particles in the flow streams
4. If electric panel is not showing the input on the mains light, check the mains supply.

58
OBSERVATION & CALCULATION

Density of water, ρW= ___________ g/cc


Density of methanol, ρM= ___________ g/cc
Molecular weight of methanol MM = 32 g/mole
Molecular weight of Water MW = 18 g/mole
Volume of water in feed VW= _____________ cc
Volume of methanol in feed VM= _____________ cc
Relative volatility α = 3.32
Packed height Z = 0.90 m
Moles of feed, F = [(VM *ρM)/MM] Methanol + [(VW *ρW)/MW] water
Mole fraction of methanol in feed xF= ______________
Mole fraction of methanol in distillate xD= _____________ (measured)
Mole fraction of methanol in residue xB= ______________ (measured)

T-x-y data for methanol-water


system
0
TC x y
100 0 0
96.4 0.02 0.134
93.5 0.04 0.23
91.2 0.06 0.304
89.3 0.08 0.365
87.7 0.1 0.418
84.4 0.15 0.517
81.7 0.2 0.579
78 0.3 0.665
75.3 0.4 0.729
73.1 0.5 0.779
71.2 0.6 0.825
69.3 0.7 0.87
67.5 0.8 0.915
66 0.9 0.958
65 0.95 0.979
64.5 1 1

Case 1: At total reflux, minimum number of stages required for the measured degree of
separation

=_______________

HETP= Z/Nm =__________

59
Case 2: At given reflux, theoretical number of stages required for the measured degree of
separation

Nt=___________(Determined by McCabe-Thiele’s method)

HETP= Z / Nt=____________

RESULTS

HETP for packed bed distillation column with Raschig rings is found to be
1. At desired reflux ratio of R=_____, HETP=______
2. At infinite reflux, minimum no of stages =________ and HETP=__________

INFERENCE

60
TERNARY LIQUID EQUILIBRIUM
Objective

To draw the binodal solubility curve for the system glacial acetic acid-benzene –
water at room temperature and pressure.

Apparatus

1. 50ccburette (3 nos)
2. 50cc test tubes (10 nos)
3. Density bottle
Chemicals

1. Glacial acetic acid.


2. Distilled water
3. Benzene
Theory

Consider the liquid-liquid extraction operation, where we are interested in separating


acetic acid from a mixture of acetic acid in water . The liquid is agitated with a liquid
such as ethyl acetate. Some of the acid but relatively less amount of water will enter the
ester phase. So the difference in miscibility of acetic acid and water in ethyl acetate and
water is taken advantage of in separating the mixture. In all such operations we see that

 there are at least three substances involved;


 there are a minimum of two immiscible liquid phases present
 the two liquid phases finally reach equilibrium when they are kept in contact with
each other for sufficient amount of time.
Study the compositions of the two phases which are in equilibrium with each other and
each of which involves three components is called ternary liquid equilibrium.

All possible compositions of three substances involved can be divided into two groups

(1) compositions in which the ternary system exists as a single phase (the three liquids are
completely miscible)

(2) composition in which the system exists in two phases. Hence in liquid extraction
design it is important to determine the following experimentally.

61
GRAPHICAL REPRESENTATION ON EQUILATERAL TRIANGULAR CO-
ORDINATES

Fig.1. Graphical representation of ternary liquid system on equilateral triangle

Suppose the components are denoted using letters A,B and,C . The same letter will be used
to indicate the quantity of a solution or mixture on a phase diagram. The concentrations of
ternary liquid systems can be plotted on equilateral triangle coordinates. It is a property of
the equilateral triangle that the sum of the perpendicular distances from any point within
the triangle to the three sides equals the altitude of the triangle. We may therefore let the
altitude represent 100% composition and the distance to the three sides the percentages or
fractions of the three components. With reference to Fig.1, each apex of the triangle
represents one of the pure components, as marked. The perpendicular distance from any
point such as K to the base AB represents the percentage of C in the mixture at K, the
distance to the base AC the percentage of B, and to the base CB the percentage of A. The
following are the some of the properties of this graphical representation.

1. If R gm of a mixture at point R is added to E gm of a mixture at E, the new mixture


can be represented by a point M which lies on the straight line RE such that
R/E= line ME/line RM=xE-xM/xM-xR ………………………………(1)

62
Where xE , xM, xR compositions of any one component in mixtures E,M,R respectively.
Similarly if a mixture at M has been removed from a mixture of composition E, the new
mixture is on the straight line EM extended in the direction away from E, and the location
of this at R is given by eqn.(1)

2. A mixture at a point D in figure (1) represent a binary mixture of A& B. To this if


C is added, the composition of the ternary mixture changes along CD.

In the Benzene(A)-Water(B)-Acetic acid(C) system, Liquid C dissolves completely in A &


B, but A & B dissolve only to a limited extent in each other. At a particular temperature
and pressure, a figure as shown in Fig.(2) can be drawn for the system. L and K represent
saturated liquid mixtures of A & B. Curve LRPEK is the binodal solubility curve. Any
mixture outside this curve will be a homogeneous solution of one liquid phase. A ternary
mixture underneath the curve, such as M, will form two insoluble saturated liquid phases
of equilibrium compositions indicated by R(A-rich) and E(B-rich). The line joining these
equilibrium compositions is called a tie line. And the point at which the tie line end is
called the plait point.

Fig.2 Ternary liquid system with C completely soluble in A&B and A&B are partially
soluble

63
Calculations

The volumes of three components taken in each experiment are converted to weight
percentage using density values.

 The composition at which the system changes from a completely miscible one to a two
phase system. If all compositions of the ternary liquid system can be represented on a
graph paper, the boundary between miscible and immicible regions can be represented
by a curve. This curve is called the binodal curve.
At given conditions of temperature and pressure composition of one phase automatically
fixes composition of other phase in equilibrium with it. Lines joining points representing
compositions of the two phases in equilibrium are called tie lines which have to be
determined experimentally.

PROCEDURE
Report the temperature at which the bimodal solubility curve is drawn. Wash the test
tubes with water, alcohol or acetone and perfectly dry it by blowing hot air. Clean the
burrettes. Distilled water is taken in burrete1, benzene in burrette 2, and glacial acetic acid
in burrette 3. Prepare nine mixtures of varying compositions in the test tubes by mixing
1cc of water with 9cc of acetic acid 2cc of water with 8 cc of acid and so on. To each
mixture, add benzene from the bottle drop by drop till a turbidity appears which indicates
light traces of separation of the new phase. Note down the volume of benzene is added to
each mixture.

Wash the test tubes well with water and some volatile liquid like alcohol or acetone and
dry it by blowing hot air. Prepare nine mixtures of acetic acid and benzene of varying
compositions by taking 1 ml benzene and 9 ml acetic acid, 2 ml benzene and 8 ml acetic
acid etc and the volumes of benzene and acetic acid taken in each are now taken down.
Add water drop by drop to each mixture till turbidity appears and note down water added.

To determine points L and K with reference to Fig.2, take 10cc of benzene in a clean dry
test tube and find out volume of water added from the burrete to make this turbid.
Similarly take 10ccs of water in a clean dry test tube and find out volume of water added
from the burrette to make this turbid. Similarly take 10ccs of water in a dry test tube and
find out the volume of benzene needed to make this turbid.

Find the specific gravity of benzene and acetic acid using specific gravity bottle.

64
OBSERVATIONS

Room temperature =

Mixture Water Acetic acid Benzene (A) Mixture Water Acetic acid Benzene (A)
No. (B) ml (C) ml No. (B) ml (C) ml
ml ml

Wt.of specific gravity bottle =

Wt.of specific gravity bottle + water =

Wt.of specific gravity bottle +acetic acid =

Wt.of specific gravity bottle + benzene =

Specific gravity of water =

Specific gravity of acetic acid =

Specific gravity of benzene =

65
The volume of three components taken in each experiment is converted to wt% using specific
gravity values.

SAMPLE CALCULATION

Wt. of water = density of water * volume of water

Wt. of acetic acid =vol. of acetic acid *density of acetic acid

Wt. of benzene = vol. of benzene *density of benzene

Wt. fraction of water =

Wt. fraction of acetic acid =

Wt. fraction of benzene =

Mix. Weight fraction Mix. No. Weight fraction

No. Water Acetic acid Benzene Water Acetic acid Benzene

66
RESULT

The binodal solubility curve for the system glacial acetic acid – benzene – water at
room temperature was plotted.

INFERENCE

67