BMS COLLEGE OF ENGINEERING

BANGALORE-19
(Autonomous College under VT!
"E#ARTMENT OF C$EMICAL ENGINEERING
MASS TRANSFER %
Laboratory Manual
L&st o' E()er&ments
Sl* No* T&tle o' t+e E()er&ment #,ge No*
1. Simple Distillation 1
2. Packed Bed Distillation 6
3.
Single Stage LiquidLiquid !traction
"
#.
Multi$Stage SolidLiquid Leac%ing
12
&.
Single Stage SolidLiquid Leac%ing
1#
6.
Multi$Stage LiquidLiquid !traction
1&
'. Steam Distillation 1"
"ATE-
E.#ERIMENT NO- 1
SIM#LE "ISTILLATION
A&m- (o )eri*y t%e +ayleig%,s equation by di**erential distillation o* t%e gi)en binary
mi!ture -.ater / met%anol system0.
T+eor/- -(o be .ritten by student on %is1%er o.n0
F&g 1- "&''erent&,l "&st&ll,t&on
(%e abo)e diagrams represent classical laboratory simple distillation2 attributed to
+ayleig% -1"330. 4eat is applied to )apori5e some o* t%e solution. (%e )apor is
condensed and *ound to contain a %ig% more )olatile component -m. ). c.0
composition -depending on amount )apori5ed0. 6o. in a small time increment -dt02
)apour o* m. ). c. composition y is gi)en o**. (%e amount o* )apor gi)en o** is dD
kmol. 7ssuming ! and y are equilibrium )alues t%roug%out t%e process2 in time
increment dt2
7pplying o)erall material balance
Moles in Moles out 8 7ccumulation
9%ere: Moles in 8 3
1
Moles out 8 dD
Moles accumulated 8 dL
3 8 dD ; dL
dD 8 dL -10
More 0ol,t&le 1om)onent (m* 0* 1! 2,l,n1e
3 / y dD 8 d -Lx0
y* dD 8 d -Lx0 8 Ldx / xdL
Substituting eq$1 in t%e abo)e equation2 .e get
y*dL 8 Ldx / xdL
xdL y*dL 8 Ldx
-x y*0 dL 8 Ldx
<
dL dx
L x y
_

,
=pon integration .e get
<
<
ln
F
W
F
W
x F
W x
x
x
dL dx
L y x
F dx
W y x

(%e last equation abo)e is kno.n as +ayleig%,s quation2 .%ere
F 8 total kmol solution to start .it%
W 8 total kmol solution le*t in bottoms
x
F
8 starting m. ). c. composition in liquid
x
W
8 *inis%ing m. ). c. composition in liquid
>* .e plot 11-y<x0 )1s x t%e area under t%e cur)e is equal to ln -F1W0
32 3 x
2
x
1
Are, under t+e 1ur0e ln (F34!
F&g* %
#ro1edure-
#re),r,t&on o' 1,l&2r,t&on 1+,rt
Mi! kno.n and )arying )olumes o* t%e gi)en mi!tures -3:232 #:162 ?:122 12:?2 16:#2
23:30 and determine t%e density o* t%e mi!ture2 using speci*ic gra)ity bottle met%od.
7lso determine t%e densities o* t%e pure components. @on)ert t%e )olume *ractions
2
into mole *ractions o* t%e more )olatile component and plot density -y$a!is0 )1s mole
*raction -x$a!is0. (%is is t%e required calibration c%art.
E()er&ment,l )ro1edure
@%arge t%e 3 necked round bottomed *lask .it% kno.n )olume o* t%e gi)en mi!ture.
7rrange t%e distillation set up as s%o.n in *ig. 1. +un cooling .ater t%roug% t%e
condenser. S.itc% on t%e %eating mantle and ensure slo. rate o* %eating -to a
temperature o* 6&
3
@0. @ontinue %eating till 31#
t%
o* t%e liquid is collected as distillate.
@ool and measure t%e )olumes o* t%e distillate and residue and *ind its densities. +ead
t%eir mole *ractions *rom t%e calibration c%art. Abtain xy data *rom t%e Perry,s
4andbook page no 13.22 '
t%
edition or ?
t%
edition and calculate 11 -y*x0.
O2ser0,t&ons ,nd C,l1ul,t&ons- Met+,nol 5A ,nd 4,ter 5 B
1. 9eig%t o* t%e empty speci*ic gra)ity bottle2 W
1
8 g
2. 9eig%t o* t%e speci*ic gra)ity bottle ; .ater2 W
2
8 g
3. 9eig%t o* t%e speci*ic gra)ity bottle ; sample2 W
3
8 g
4. 9eig%t o* .ater 8 W
2
W
1
8 g
5. 9eig%t o* sample 8 W
3
W
1
8 g
6. Density o* .ater 8
2 1
2 1
W W
Y
W W
1

]
, Bg1m
3
9%ere C is t%e density o* .ater obtained *rom Perry 4and Book
7. Density o* mi!tures8
3 1
2 1
Density o* .ater
W W
W W
1

]
, Bg1m
3
?. Moles o* met%anol 8 -Dolume E density1 mol. .t.0 o* met%anol
". Moles o* .ater 8 -Dolume E density1 mol. .t.0 o* .ater
13. Moles o* *eed F 8 -Dolume E density1mol. .t.0
met%anol
; -Dolume E density1mol.
.t.0
.ater
11. Mole Fraction o* Met%anol2
x
F
8 moles o* met%anol 1 moles o* *eed
3
T,2le 1- @alibration c%art *or met%anol .ater mi!tures
Sl.
6o.
Dolume
o* .ater
in ml
Dolume o*
met%anol in
ml
9eig%t o*
speci*ic
gra)ity
bottle ;
mi!ture
9eig%t o*
t%e mi!ture
in g
Density
o* t%e
mi!ture
g1cc
Mole
*raction o*
met%anol2
x
1 33 23
2 3# 16
3 3? 12
# 12 3?
& 16 3#
6 23 33
T,2le %- quilibrium Data *rom Perry,s 4and book
T
x
y*
11y<
x
12. Dolume o* distillate2 V
D
8 m
3
13. 9eig%t o* t%e speci*ic gra)ity bottle ; distillate2 W
4
8 g
1#. Density o* distillate2
D
in -Bg1m
3
0 8 -9
#
9
1
0 1 )olume o* t%e speci*ic gra)ity
bottle
1&. Mole *raction o* distillate2 x
D
8 to be obtained *rom t%e calibration c%art based on
density o* distillate
16. 7)erage molecular .eig%t o* t%e distillate2 M
D,avg
8 !
D
E -Mol. .t.0
met%anol
; -1 x
D
0
E -Mol. .t.0
.ater

1'. Moles o* distillate2 D 8 V
D
E
D
1 M
D,avg
1?. Dolume o* residue V
R
8 m
3
1". 9eig%t o* t%e speci*ic gra)ity bottle ; reside2 W
&
8 g
#
23. Density o* residue2

.
in Bg1m
3
8 - W
&
W
1
0 1 )olume o* t%e speci*ic gra)ity bottle
21.

Mole *raction o* residue2
x
w

8 to be obtained *rom t%e calibration c%art based on density o*

residue
22.

Moles o* residue 2 W 8 F D
+.4.S. o* +ayleig%,s equation 8
<
F
W
x
x
dx
y x

L.4.S. o* +ayleig%,s equation 8 ln -F1W0

Result- L.4.S. 8 +.4.S.
4ence +ayleig%,s equations )eri*ied.
&
E()er&ment No- % ",te-163%317
#,18ed Bed "&st&ll,t&on
A&m- (o *ind 4eig%t qui)alent to a (%eoretical Plate -4(P0 o* a Packed distillation
column.
A)),r,tus- Packed distillation column setup2 separating *unnel2 speci*ic gra)ity bottle.
T+eor/: Distillation is a met%od o* separating t%e components o* a solution .%ic%
depends upon t%e distribution o* t%e substance bet.een a gas and a liquid p%ase2 applied
to cases .%ere all compounds are present in bot% p%ases. 7 distillation column %as a re$
boiler2 condenser and a column. >n t%is e!periment2 some crucial parameters *or
distillation suc% as re*lu! ratio are in)estigated2 di**erent re*lu! ratio )alues are used *or
eac% step and e**ect o* re*lu! ratio c%ange on parameters is researc%ed and t%e %eig%t o*
column is calculated t%eoretically by using Mc@abe (%iele met%od. Packed columns are
used *or distillation2 gas absorption and liquid$liquid e!traction.
(%e gas$liquid contact in a packed column is continuous2 not stage$.ise2 as in a
plate column. (%e liquid *lo.s do.n in t%e column o)er a packing sur*ace and t%e )apor
-or t%e gas0 mo)es counter$currently2 up t%e column. (%e per*ormance o* a packed
column is )ery dependent on t%e maintenance o* good liquid and gas distribution t%roug%
t%e packed bed2 and t%is is an important consideration in packed column design.
(%ere are some ad)antages and disad)antages *or t%e plate and t%e packed columns.
1. Plate columns can be designed to %andle a .ider range o* liquid and gas *lo. rates
t%an packed columns.
2. Packed columns are not suitable *or )ery lo. liquid *lo. rates.
3. (%e e**iciency o* a plate can be predicted more accurately t%an t%e equi)alent in terms
o* Packing -HETP or HTU0.
#. For corrosi)e liquids a packed column .ill usually be c%eaper t%an t%e equi)alent plate
column.
&. (%e liquid %old$up is lo.er in a packed column t%an in a plate column. (%is can be
important .%en t%e %old$up o* to!ic or *lammable liquids must be kept as small as
possible *or sa*ety reasons.
6. Packed columns are more suitable *or %andling *oaming systems.
'. (%e pressure drop can be lo.er in a packed column t%an t%e equi)alent plate column.
#ro1edure-
#re),r,t&on o' 1,l&2r,t&on 1+,rt:
Mi! kno.n and )arying )olumes o* t%e gi)en mi!tures -3:232 #:162 ?:122 12:?2 16:# and
23:30 and determine t%e density o* t%e mi!ture2 using speci*ic gra)ity bottle met%od. 7lso
determine t%e densities o* t%e pure components. @on)ert t%e )olume *ractions into mole
*ractions o* t%e more )olatile component and plot density -y$a!is0 )1s mole *raction -!$
a!is0. (%is is t%e required calibration c%art.
E()er&ment,l )ro1edure
6
7rrange t%e e!perimental set up. 7llo. cooling .ater to *lo. t%roug% t%e condenser*
@%arge t%e +ound Bottom *lask .it% #33ml o* t%e gi)en sample -Met%anol$9ater mi! 8
6&:3&0 a*ter *inding its speci*ic gra)ity. S.itc% on t%e %eating mantle and %eat at constant
steady state %eating -to a temperature o*
3
@0. 7llo. t%e system to attain equilibrium
-(ill 31#
t%
o* t%e sample is distilled0. (%en take a small quantity o* t%e distillate and
residue2 cool and *ind out t%eir speci*ic gra)ity. 6ote t%e mole *raction o* t%e distillate
and t%e residue *rom t%e calibration c%art. 6ote t%e t$!$y data *or met%anol .ater
mi!tures *rom t%e %and book *or calculation o* relati)e )olatilities.
O2ser0,t&ons ,nd C,l1ul,t&ons- (Met+,nol 5A ,nd 4,ter 5 B!
1. 9eig%t o* t%e empty speci*ic gra)ity bottle2 W
1
8 1?.'1 g
2. 9eig%t o* t%e speci*ic gra)ity bottle ; .ater2 W
2
8 2?.'1 g
3. 9eig%t o* t%e speci*ic gra)ity bottle ; sample2 W
3
8 26.6# g
4. 9eig%t o* .ater 8 W
2
W
1
8 13.31 g
5. 9eig%t o* sample 8 W
3
W
1
8 '."# g
6. Density o* .ater 8
2 1
2 1
W W
Y
W W
1

]
8 ""'.3#& Bg1m
3
9%ere C is t%e density o* .ater obtained *rom Perry 4and Book.
7. Density o* met%anol 8
3 1
2 1
Density o* .ater
W W
W W
1

]
8'"3.?62? Bg1m
3
?. Moles o* met%anol 8 -Dolume E density1 mol. .t.0 o* met%anol8 3.336#2&
". Moles o* .ater 8 -Dolume E density1 mol. .t.0 o* .ater 8 3.33''&#
13. Mole *raction o* met%anol in t%e *eed *rom calibration c%art2 x
F
8 3.&2
11. Mole *raction o* met%anol in t%e distillate *rom calibration c%art2 x
D
8 3."?
12. Mole *raction o* met%anol in t%e residue *rom calibration c%art2 x
W
8 3.#?
T,2le 1- @alibration c%art *or met%anol .ater mi!tures
Sl.
6o.
Dolume o*
.ater in ml
Dolume o*
met%anol in ml
9eig%t o*
speci*ic
gra)ity bottle
; mi!ture
9eig%t o*
t%e mi!ture
in g
Density
o* t%e
mi!ture
Mole
*raction
o*
met%anol2
x
1 33 23 26.6# '.?# '"3.62? 1
'
2 3# 16 2'.3& ?.6& ?61.&? 3.6#
3 3? 12 2'.'# ".3# "33.#2 3.#
# 12 3? 2?.12 ".#2 "32.2'? 3.22"
& 16 3# 2?.#3 ".'3 "6".1& 3.1333
6 23 33 2?.'1 13.31 ""'.3# 3
T,2le 1- Txy data *rom 4and Book
( G C H
133 3 3 3
"6.# 3.32 3.13# '.'
"3.& 3.3# 3.23 '.26
"1.2 3.36 3.33# 6."2
?".3 3.3? 3.36& 6.6'
?'.' 3.1 3.#1? 6.#6
?#.# 3.1& 3.&1' 6.33
?1.' 3.2 3.&'" &.&
'? 3.3 3.66& #.63
'&.3 3.# 3.'2" 3."&
'3.1 3.& 3.''" 3.&2#
'1.2 3.6 3.?2& 3.1#
6".3 3.' 3.?'3 2.?'
6'.& 3.? 3."1& 2.6"
66 3." 3."&? 2.&3
6& 3."& 3."'6 2.1#
6#.& 1 1 $

a)
8 I
1
E
2
E
3
E
#
JnK
11n
8#.2#"
?
Met+od 1- Fenske,s quation
13.
av
W
W
D
D
m
x
x
x
x
N
log
1
.
1
log
1

,
_

+
8 #
Met+od %- (%e number o* t%eoretical plates can also be calculated by Mc@abe (%iele
met%od *or t%e condition o* (otal +e*lu!. 8 3
-Feed is unsaturated liquid0
1#. 4eig%t equi)alent to a t%eoretical plate2 4..(.P. 8 4eig%t o* packing16umber o*
t%eoretical plates.
4eig%t o* packing 8 #33 mmn
Results:
4..(.P by Fenske,s met%od 8 133mm
4..(.P by Mc@abe (%iele met%od 8133mm
"
13
E()er&ment No- 9 ",te-
S&ngle St,ge L&:u&d-L&:u&d E(tr,1t&on
A&m- (o determine t%e percentage reco)ery o* acetic acid *rom a solution o* .ater$
acetic acid using et%yl acetate as a sol)ent by single stage e!traction.
T+eor/- Liquid/liquid e!traction also kno.n as sol)ent e!traction and partitioning2 is a
met%od to separate compounds based on t%eir relati)e solubilities in t.o di**erent
immiscible liquidL1Ms2 usually .ater and an organic sol)ent. >t is an e!traction o* a
substance *rom one liquid into anot%er liquid p%ase. Liquid/liquid e!traction is a basic
tec%nique in c%emical laboratories2 .%ere it is per*ormed using a separatory *unnel. (%is
type o* process is commonly per*ormed a*ter a c%emical reaction as part o* t%e .ork$up.
(%e term partitioning is commonly used to re*er to t%e underlying c%emical and
p%ysical processes in)ol)ed in liquid/liquid e!traction but may be *ully synonymous. (%e
term sol)ent e!traction can also re*er to t%e separation o* a substance *rom a mi!ture by
pre*erentially dissol)ing t%at substance in a suitable sol)ent. >n t%at case2 a soluble
compound is separated *rom an insoluble compound or a comple! matri!.
Ion e(1+,nge me1+,n&sm- 7not%er e!traction mec%anism is kno.n as t%e ion e!c%ange
mec%anism. 4ere2 .%en an ion is trans*erred *rom t%e aqueous p%ase to t%e organic
p%ase2 anot%er ion is trans*erred in t%e ot%er direction to maintain t%e c%arge balance.
(%is additional ion is o*ten a %ydrogen ionN *or ion e!c%ange mec%anisms2 t%e distribution
ratio is o*ten a *unction o* p4
Ion ),&r e(tr,1t&on- >t is possible by care*ul c%oice o* counter ion to e!tract a metal. For
instance2 i* t%e nitrate concentration is %ig%2 it is possible to e!tract americium as an
anionic nitrate comple! i* t%e mi!ture contains a lipop%ilic quaternary ammonium salt.
T/)es o' ,:ueous t;o-)+,se e(tr,1t&ons-
#ol/mer<)ol/mer s/stems- >n a Polymer/polymer system2 bot% p%ases are generated by
a dissol)ed polymer. (%e %ea)y p%ase .ill generally be Polyet%ylene glycol -PO02 and
t%e lig%t p%ase is generally a polysacc%aride. (raditionally2 t%e polymer used is de!tran.
4o.e)er2 de!tran is relati)ely e!pensi)e2 and researc% %as been e!ploring using less
e!pensi)e polysacc%arides to generate t%e lig%t p%ase.
#ol/mer<s,lt s/stems- 7queous t.o$p%ase systems can also be generated by introducing
a %ig% concentration o* salt to a polymer solution. (%e polymer p%ase used is generally
PO. Oenerally2 a kosmotropic salt2 suc% as 6a3PA# is used2 %o.e)er PO/6a@l systems
%a)e been documented .%en t%e salt concentration is %ig% enoug%.
Ion&1 l&:u&ds- >onic liquids are ionic compounds .it% lo. melting points. 9%ile t%ey are
not tec%nically aqueous2 recent researc% %as e!perimented .it% using t%em in an
e!traction t%at does not use organic sol)ents.
A))l&1,t&on- Sol)ent e!traction is used in nuclear reprocessing2 ore processing2 t%e
production o* *ine organic compounds2 t%e processing o* per*umes2 t%e production o*
)egetable oils and biodiesel2 and ot%er industries.
#ro1edure: !traction is studied *or t%e system o* 7cetic acid -Solute02 9ater
-@arrier0 and t%yl acetate -Sol)ent0.
#re),r,t&on o' C,l&2r,t&on 1+,rt 'or R,''&n,te )+,se-
Prepare t%e mi!tures o* 3:232 #:162 ?:122 12:?2 16:# and 23:3 )olume proportions o*
.ater and acetic acid respecti)ely and determine t%eir densities. 7lso determine t%e
densities o* pure .ater and acetic acid. @on)ert t%e )olume ratios into mass *ractions
o* acetic acid in .ater. Plot a grap% o* density -y$a!is0 )1s mass *raction -!$a!is0. (%is
is t%e calibration c%art *or t%e +a**inate p%ase.
11
#re),r,t&on o' 1,l&2r,t&on 1+,rt 'or e(tr,1t )+,se-
Prepare t%e mi!tures o* 3:232 #:162 ?:122 12:?2 16:# and 23:3 )olume proportions o*
et%yl acetate and acetic acid and determine t%eir density. 7lso determine t%e densities
o* pure et%yl acetate and acetic acid. @on)ert t%e )olume ratios into mass *raction o*
acetic acid in et%yl acetate. Plot a grap% o* density -y$a!is0 )1s mass *raction -!$a!is0.
(%is is t%e calibration c%art *or t%e e!tract p%ase.
S&ngle st,ge o)er,t&on-
Mi! &3 ml o* .ater and 13 ml o* acetic acid and pour into t%e stoppered *lask. (o t%is
mi!ture add 1&3 ml o* et%yl acetate and s%ake it *or 33 min in a mec%anical s%aker.
7*ter 33 min2 separate t%e ra**inate layer -.ater$ acetic acid0 and e!tract layer -et%yl
acetate / acetic acid 0 using a separating *unnel. 6ote do.n t%e density o* ra**inate
layer and e!tract layer. 6ote do.n t%e mass *ractions using t%eir respecti)e
calibration c%arts.
O2ser0,t&on ,nd C,l1ul,t&ons-
= Negle1t&ng t+e solu2&l&t/ o' Et+/l ,1et,te &n ;,ter>
Solute 8 7cetic acid -@0
Sol)ent 8 t%yl acetate -B0
@arrier 8 9ater -70
1. 9eig%t o* t%e empty speci*ic gra)ity bottle2 W
1
8 g
2. 9eig%t o* t%e speci*ic gra)ity bottle ; .ater2 W
2
8 g
3. 9eig%t o* t%e speci*ic gra)ity bottle ; sample2 W
3
8 g
4. 9eig%t o* .ater 8 W
2
W
1
8 g
5. 9eig%t o* sample 8 W
3
W
1
8 g
6. Density o* .ater 8
2 1
2 1
W W
Y
W W

, Bg1m
3
.%ere Y is t%e density o* .ater taken *rom Perry.
7. Density o* sample 8
3 1
2 1
Density o* .ater
W W
W W

, Bg1m
3
T,2le 1- @alibration c%art o* +a**inate p%ase
Sl.
6o.
Dolume
o* .ater
in ml
Dolume
o* acetic
acid in ml
9eig%t o*
speci*ic
gra)ity bottle
; sample
9eig%t
o*
sample
in g
Density o*
t%e sample
Mass *raction
o* acetic acid
in ra**inate
1 33 23
2 3# 16
3 3? 12
# 12 3?
& 16 3#
6 23 33
12
T,2le %- @alibration c%art o* !tract p%ase
Sl.
6o
.
Dolume
o* et%yl
acetate in
ml
Dolume
o* acetic
acid in ml
9eig%t o*
speci*ic
gra)ity bottle
; sample
9eig%t o*
sample
Density
o* t%e
sample
Mass
*raction o*
acetic acid
in !tract
1 33 23
2 3# 16
3 3? 12
# 12 3?
& 16 3#
6 23 33
?. Mass o* Feed2 F 8
C C
V V +
2 Bg
". Mass *raction o* @ in *eed2 x
F
8 Abtained *rom calibration c%art o* +a**inate
13. Mass *raction o* @ in !tract2 y
E
8 Abtain *rom calibration c%art using density o*
!tract
11. Dolume o* +a**inate

2 V
R
8
12. Dolume o* !tract2 V
E
8
13. Mass o* +a**inate2 -R0 8V
R
E
R

8
1#. Mass o* !tract2 -E

0 8V
E
E
E

8
1&. Mass *raction o* @ in +a**inate2 x
R
8 Abtain *rom calibration c%art using density
o* ra**inate
16. P @ e!tracted -based on +a**inate0 8
( )
in Feed in +
in Feed
133
C C
C

8
( )
F
F
!
133
! F
R
F x R

1'. P @ e!tracted -based on !tract0 8
( )

in Feed
y Mass o*
133
C

8
( )
( )
F
133
! F
E
y E 1

]
Result: (%e percentage e!traction o* acetic acid *rom acetic acid$ .ater mi!ture
using et%yl acetate as sol)ent in single stage isQQQQQQP based on +a**inate and is
QQQQQQ P based on !tract
13
E()er&ment No- 7 ",te-
Mult& st,ge Sol&d L&:u&d Le,1+&ng
A&m- (o estimate percentage leac%ing o* o!alic acid *rom sand using .ater as a
sol)ent using t%ree stages cross current operation.
T+eor/- -(o be .ritten by student on %is1%er o.n0
#ro1edure-
Standardi5ation o* solutions: Standardi5e 6aA4 -3.1 60 solution using o!alic acid
-3.1 60. =se p%enolp%t%alein indicator.
T+ree St,ge O)er,t&ons-
St,ge 1- (ake 133 g o* .et sand in a 2&3 ml beaker and add 2 g o* o!alic acid. Mi!
.ell and add &3 ml .ater. Stir t%oroug%ly *or 13 min and allo. t%e solids to settle.
Decant t%e clear liquid and titrate 13 ml o* t%e liquid .it% t%e standardi5ed 6aA4
solution using p%enolp%t%alein indicator and note do.n t%e titrate )alue.
St,ge %- (o t%e sand add anot%er &3 ml o* .ater. Stir t%oroug%ly *or 13 min and allo.
t%e solids to settle. Decant t%e clear liquid and titrate 13 ml o* t%e liquid .it% t%e
standardi5ed 6aA4 solution using p%enolp%t%alein indicator and note do.n t%e titrate
)alue.
St,ge 9- (o t%e sand add anot%er &3 ml o* .ater. Stir t%oroug%ly *or 13 min and allo.
t%e solids to settle. Decant t%e clear liquid and titrate 13 ml o* t%e liquid .it% t%e
standardi5ed 6aA4 solution using p%enolp%t%alein indicator and note do.n t%e titrate
)alue.
O2ser0,t&on ,nd C,l1ul,t&ons-
9eig%t o* o!alic acid taken2 W
i
8 2 g
St,ge 1- -133 g sand ; 2 g o!alic acid0 ; -&3 ml .ater0
T,2ul,r 1olumn
Sl. 6o. >nitial )olume in burette
in ml
Final )olume in burette
in ml
Dol. o* 6aA4 rundo.n
in ml
1
2
7)erage )olume o* 6aA4 rundo.n
Dolume o* 6aA4 consumed -run do.n *rom burette0
1
V
8
6ormality o* t%e sample2 N
1
8
( )
1
13
Na!H
V N

1#
Ruantity o* o!alic acid leac%ed 8
1
1
63
&3
1333
N
W


' ;

St,ge %-
T,2ul,r 1olumn
Sl. 6o. >nitial )olume in burette
in ml
Final )olume in burette
in ml
Dol. o* 6aA4 rundo.n
in ml
1
2
7)erage )olume o* 6aA4 rundo.n
Dolume o* 6aA4 consumed -run do.n *rom burette0
2
V
8
6ormality o* t%e sample2 N
2
8
( )
2
13
Na!H
V N

Ruantity o* o!alic acid leac%ed 8
2
2
63
&3
1333
N
W


' ;


St,ge 9-
T,2ul,r 1olumn
Sl. 6o. >nitial )olume in burette
in ml
Final )olume in burette
in ml
Dol. o* 6aA4 rundo.n
in ml
1
2
7)erage )olume o* 6aA4 rundo.n
Dolume o* 6aA4 consumed -run do.n *rom burette02
3
V
8
6ormality o* t%e sample2 N
3
8
( )
3
13
Na!H
V N

Ruantity o* o!alic acid leac%ed 8
3
3
63
&3
1333
N
W


' ;


A)erall Percentage Leac%ing 8
1 2 3
133
"
W W W
W
+ +

' ;

Result- Percentage o* o!alic acid leac%ed *rom sand using .ater as a sol)ent in a
t%ree stage cross current operation is QQQQQQQQQP.
1&
E()er&ment No- ? ",te-1?3%317
S&ngle st,ge Sol&d L&:u&d Le,1+&ng
A&m- (o estimate percentage leac%ing o* o!alic acid *rom sand using .ater as a
sol)ent.
T+eor/- Leac%ing is a liquid$solid operation. (%e t.o p%ases are in intimate contact2
t%e solutes can di**use *rom t%e solid to t%e liquid p%ase2 .%ic% causes a separation o*
t%e components originally in t%e solid. 7 special leac%ing process2 .%en an
undesirable component is remo)ed *rom a solid .it% .ater2 is called .as%ing.
(%e *ollo.ing *igure s%o.s a single$stage leac%ing process .%ere D is kg1% o*
o)er*lo. solution .it% composition !
7
and L is t%e kg1% o* liquid in t%e slurry
solution .it% composition y
72
based on a gi)en *lo. rate B2 kg1% o* dry solute$*ree
solid.
By doing material balances2 .e %a)e (otal solution
-7;@0: L
3
; D
2
8 L
1
; D
1
8 M
-70 : L
3
y
73
;D
2
!
72
8 L
1
y
71
;D
1
!
71
8 M!
7M
-B0 : B 8L
3
6
3
;38L
1
6
1
;38 M6
M
7 balance on @ is not needed since !
7
; !
@
8 1 and y
7
; y
@
8 1 2.%ere M is t%e
total *lo. rate in kg -7;@01%2 !
7M
and 6M are t%e coordinates o* t%is point M.
>* L
3
entering is t%e *res% solid *eed to be leac%ed .it% no sol)ent @ present2 it .ould
be located abo)e t%e 6 )ersus y line in t%e abo)e *igure
Leac%ing is .idely used in t%e biological and *ood processing industries2 suc% as
t%e separation o* sugar *rom sugar beets .it% %ot .ater2 t%e e!traction o* oils *rom
peanuts2 soybeans2 sun*lo.er seeds2 cotton seeds2 and %alibut li)ers. >n
p%armaceutical industry2 many products are obtained by leac%ing plant roots2 lea)es2
and stems.
#ro1edure-
Standardi5ation o* solutions: Standardi5e 6aA4 -3.1 60 solution using o!alic acid
-3.1 60. =se p%enolp%t%alein indicator.
S&ngle St,ge O)er,t&on-
(ake 133 g o* .et sand in a 2&3 ml in a beaker and add 2 g o* o!alic acid. Mi! .ell
and add 1&3 ml .ater. Stir t%oroug%ly *or 33 min and allo. t%e solids to settle.
Decant t%e clear liquid and titrate 13 ml o* t%e liquid .it% t%e standardi5ed 6aA4
16
solution using p%enolp%t%alein indicator and note do.n t%e titrate )alue.
O2ser0,t&on ,nd C,l1ul,t&ons-
S&ngle st,ge-
9eig%t o* o!alic acid taken2 W
i
8 2 g
T,2ul,r 1olumn
Sl. 6o. >nitial )olume in burette
in ml
Final )olume in burette
in ml
Dol. o* 6aA4 rundo.n
in ml
1 3 13.# 13.#
2 13.# 23." 13.&
7)erage )olume o* 6aA4 rundo.n 13.#&
Dolume o* 6aA4 consumed -run do.n *rom burette0 8 13.#&ml
6ormality o* 6aA42 6
6aA4
8 3.3"&6" 6
6ormality o* t%e sample2 N
sample
8
( )
13
Na!H Na!H
V N
8 3.23" 6
Ruantity o* o!alic acid leac%ed2 W 8
( )
63
1&3
1333
#am$%&
N

' ;


8 1."?g
Percentage o* o!alic acid leac%ed 8
133
"
W
W
_

,
8 "".336P S 133P
Result- Percentage o* o!alic acid leac%ed *rom sand using .ater as a sol)ent in a
single stage is 133P.
1'
E()er&ment No- @ ",te-
Mult& St,ge L&:u&d-L&:u&d E(tr,1t&on
A&m (o determine t%e percentage reco)ery o* acetic acid *rom a solution o* .ater$
acetic acid using et%yl acetate as a sol)ent by multi stage e!traction.
T+eor/ -(o be .ritten by student on %is1%er o.n0
#ro1edure
!traction is studied *or t%e system o* 7cetic acid -Solute02 9ater -@arrier0 and t%yl
acetate -Sol)ent0.
#re),r,t&on o' C,l&2r,t&on 1+,rt 'or R,''&n,te )+,se
Prepare t%e mi!tures o* 3:232 #:162 ?:122 12:?2 16:# and 23:3 )olume proportions o*
.ater and acetic acid respecti)ely and determine t%eir densities. 7lso determine t%e
densities o* pure .ater and acetic acid. @on)ert t%e )olume ratios into mass *ractions
o* acetic acid in et%yl acetate. Plot t%e density on y$a!is and mass *raction on !$a!is.
(%is is t%e calibration c%art *or t%e +a**inate p%ase.
#re),r,t&on o' 1,l&2r,t&on 1+,rt 'or e(tr,1t )+,se
Prepare t%e mi!tures o* 3:232 #:162 ?:122 12:?2 16:# and 23:3 )olume proportions o*
et%yl acetate and acetic acid and determine t%eir density. 7lso determine t%e densities
o* pure et%yl acetate and acetic acid. @on)ert t%e )olume ratios into mass ratios o*
acetic acid in et%yl acetate. Plot t%e density -on y$a!is0 and mass *raction -on !$a!is0.
(%is is t%e calibration c%art *or t%e e!tract p%ase.
Mult& st,ge o)er,t&on
St,ge 1- Mi! &3 ml o* .ater and 13 ml o* acetic acid and pour into t%e stoppered
*lask. (o t%is mi!ture add &3 ml o* et%yl acetate and s%ake it *or 13 min in a
mec%anical s%aker. 7*ter 13 min2 separate t%e ra**inate -.ateracetic acid0 and e!tract
layers -et%yl acetate / acetic acid0 using a separating *unnel. Measure t%e )olume o*
t%e e!tract layer. 6ote do.n t%e density o* t%e e!tract layer. 6ote do.n its mass
*raction using its calibration c%art.
St,ge %- (ake t%e ra**inate layer o* stage$1. 7dd &3 ml o* et%yl acetate and s%ake it
*or 13 min in a mec%anical s%aker. 7*ter 13 min2 separate t%e ra**inate -.ater$ acetic
acid0 and e!tract layers -et%yl acetate / acetic acid0 using a separating *unnel.
Measure t%e )olume o* t%e e!tract layer. 6ote do.n t%e density o* t%e e!tract layer.
6ote do.n its mass *raction using its calibration c%art.

St,ge 9- (ake t%e ra**inate layer o* stage$2. 7dd &3ml o* et%yl acetate and s%ake it *or
13 min in a mec%anical s%aker. 7*ter 13 min2 separate t%e ra**inate -.ateracetic
acid0 and e!tract layers -et%yl acetate/acetic acid0 using a separating *unnel. Measure
t%e )olume o* t%e e!tract layer. 6ote do.n t%e density o* t%e e!tract layer. 6ote do.n
its mass *raction using its calibration c%art. Measure t%e )olume o* t%e ra**inate layer.
6ote do.n t%e density o* t%e ra**inate layer. 6ote do.n its mass *raction using its
calibration c%art.
1?
O2ser0,t&on ,nd C,l1ul,t&ons
= Negle1t&ng t+e solu2&l&t/ o' Et+/l ,1et,te &n ;,ter>
Solute 8 7cetic acid -@0
Sol)ent 8 t%yl acetate -B0
@arrier 8 9ater -70
1. 9eig%t o* t%e empty speci*ic gra)ity bottle2 W
1
8 g
2. 9eig%t o* t%e speci*ic gra)ity bottle ; .ater2 W
2
8 g
3. 9eig%t o* t%e speci*ic gra)ity bottle ; sample2 W
3
8 g
4. 9eig%t o* .ater 8 W
2
W
1
8 g
5. 9eig%t o* sample 8 W
3
W
1
8 g
6. Density o* .ater 8
2 1
2 1
W W
Y
W W
1

]
, kg1m
3
.%ere2 Y is t%e density o* .ater at room temperature obtained *rom Perry 4and
Book.
7. Density o* sample 8
3 1
2 1
Density o* .ater
W W
W W
1

]
, kg1m
3
T,2le 1- @alibration c%art o* +a**inate p%ase
Sl.
6o.
Dolume
o* .ater
in ml
Dolume
o* acetic
acid in ml
9eig%t o*
speci*ic
gra)ity bottle
; sample
9eig%t
o*
sample
in g
Density o*
t%e sample
Mass *raction
o* acetic acid
in ra**inate
1 33 23
2 3# 16
3 3? 12
# 12 3?
& 16 3#
6 23 33
T,2le %- @alibration c%art o* !tract p%ase
Sl. Dolume Dolume 9eig%t o* 9eig%t o* Density Mass
1"
6o
.
o* et%yl
acetate in
ml
o* acetic
acid in ml
speci*ic
gra)ity bottle
; sample
sample
in g
o* t%e
sample
*raction o*
acetic acid
in !tract
1 33 23
2 3# 16
3 3? 12
# 12 3?
& 16 3#
6 23 33
St,ge 1
Mass o* Feed2 F 8
' '
V V +
8 Bg
Dolume o* !tract
1
2 V
E1
8
Mass *raction o* @ in *eed2 x
F
8 Abtained *rom calibration c%art o* +a**inate
Mass *raction o* @ in !tract
1
2 y
E1
8 Abtain *rom calibration c%art using density o*
!tract
1
.
Mass o* !tract
1
2 E
1
8 V
E1
E
1 E

8
St,ge %
Dolume o* !tract
2
2 V
E2
8
Mass o* !tract
2
2 E
2
8 D
2
E
2
E

Mass *raction o* @ in !tract

2
2 y
2
8 Abtain *rom calibration c%art using density o*
!tract
2
.
St,ge-9
Dolume o* +a**inate
3
2 V
R3
8
Mass o* +a**inate
3
8 V
R3
E
3
R

8
Mass *raction o* @ in +a**inate
3
2 !
+3
8 Abtain *rom calibration c%art using density o*
+a**inate
3
.
Dolume o* !tract
3
2 V
E3
8
Mass o* !tract
3
8 V
E3
E
3
E

Mass *raction o* @ in !tract

3
2 y
3
8 Abtain *rom calibration c%art using density o*
!tract
3
.

P @ e!tracted -based on +a**inate0 8
( )
3
in Feed in +
in Feed
133
C C
C

8
( )
3
3 3
Mass o* Feed
133
Mass o* Feed
F R R R
F
x x V
x

P @ e!tracted -based on !tract0 8

( ) ( ) ( )
1 1 2 2 3 3
in Feed
Mass o* Mass o* Mass o*
133
E E E
y E y E y E
C
+ + 1
]

23
Result: (%e percentage e!traction o* acetic acid *rom acetic acid$.ater mi!ture using
et%yl acetate as sol)ent in 3$stages isQQQQQQQQQ P based on +a**inate and
QQQQQQQQQP based on !tract.
21
"ATE-
E.#ERIMENT NO- A
Ste,m "&st&ll,t&on
AIM- (o )eri*y t%e principal o* immiscible liquid mi!ture boiling T *inding )apori5ing
e**iciency and t%ermal e**iciency.
A##ARRATS- +ound bottom *lask2 +e*lu! condenser2 (%ermostat2 Measuring Uar2
conical *lask2 Speci*ic gra)ity bottles.
T$EORB- -(o be .ritten by student on %is1%er o.n0
#ROCE"RE-
1. 1&3 ml o* pure nitroben5ene is taken in around bottom *lask.
2. 7ll t%e *ittings are connected and t%e .ater is circulated in t%e condenser. (%e
t%ermometer is arranged in t%e pockets pro)ided.
3. Steam is generated in t%e steam boilers and is bubbled in.
#. (%e nitroben5ene )apors are condensed and collected in a beaker.
&. 9%en su**icient distillate is collected -&33 ml0 t%e operation is stopped.
6. (%e temperature at .%ic% t%e system boils during steam distillation is noted.
'. (%e distillate is allo.ed to settle in a separating *unnel2 and t%e )olumes o* .ater and
nitroben5ene are measured.
?. Similarly2 t%e residue is also cooled and trans*erred to a separating *unnel and t%e
)olumes o* .ater and nitroben5ene are measured.
". (%en t%e speci*ic gra)ity o* eac% layer in t%e distillate and residue are calculated.
CALCLATION
Dapor pressure )s. temperature *or niroben5ene is a)ailable in Perry %andbook page 2$'1.
nt%alpy o* nitroben5ene at normal boiling point is gi)en as 33.?' BV1Bg.
9atson equation to *ind ent%alpy o* nitroben5ene at t%e boiling temperature -met%od 20.
O2ser0,t&ons ,nd Formul,e
1. 9t. o* speci*ic gra)ity bottle 8 g
2. Dolume o* Feed 8 ml
3. 9eig%t o* pure nitroben5ene taken in speci*ic gra)ity bottle 8 g
#. 9eig%t o* pure .ater taken in speci*ic gra)ity bottle 8 g
&. Speci*ic gra)ity o* pure nitroben5ene 8
6. !perimental distillation temperature2 T
d &x$
8
o
@
"&st&ll,te-
'. Dolume o* nitroben5ene2 V
1
8 ml
?. Dolume o* .ater2 V
2
8 ml
". 9eig%t o* nitroben5ene taken in speci*ic gra)ity bottle 8 g
13. 9eig%t o* .ater taken in speci*ic gra)ity bottle 8 g
22
11. Speci*ic gra)ity o* nitroben5ene2 (
1
8
12. Speci*ic gra)ity o* .ater2 (
2
8
Res&due-
13. Dolume o* nitroben5ene2 V
3
8 ml
1#. Dolume o* .ater2 V
#
8 ml
1&. 9eig%t o* nitroben5ene taken in speci*ic gra)ity bottle 8 g
16. 9eig%t o* .ater taken in speci*ic gra)ity bottle 8 g
1'. Speci*ic gra)ity o* nitroben5ene2 (
3
8
1?. Speci*ic gra)ity o* .ater2 (
#
8
1". m
1
8 V
1
E (
1
23. m
2
8 V
2
E (
2
21. m
3
8 V
3
E (
3
22. m
#
8 V
#
E (
#
23. Steam requirement8 -m
2
; m
#
01m
1
2 kg steam1kg nitroben5ene
2#. Steam pressure2 P
#
8 bar
2&. Saturation temperature2 T
#
at P
#
8
o
@
26. Latent %eat o* )apori5ation at T
#
8
#
8 kV1kg
2'. Latent %eat o* )apori5ation at T
d &x$
8
W"2
o
@
8

kV1kg
T,2le 1- Dapor pressure data *or .aternitroben5ene system -*rom Perry0
(emperature
-
o
@0
Dapor Pressure
o*
6itroben5ene2 P

-mm 4g0
Dapor Pressure
o*
9ater2 P
)
-mm 4g0
P
T
P
)
-mm 4g0
9%ere2 P
T
8 ambient pressure 8 13132& Pa
2?. 7mbient temperature8 T
a
8
o
@
$e,t In)ut-
2". -m
2
; m
#
0 E LC
$w
-T
#
T
a
0 ; *
#
M2 kV
9%ere2 C
$w
is taken at -T
#
; T
a
012
23
$e,t Out)ut
Res&due-
33. m
3
E C
$N)
E -T
d&x$
/ T
a
0 ; m
#
E C
$w
E -T
d&x$
T
a
02 kV
9%ere2 C
$w
is speci*ic %eat o* .ater taken at T
avg
8 -T
d&x$
; T
a
0122 kV1kg
o
@
C
$N)
is speci*ic %eat o* nitroben5ene taken at T
avg
8 -T
d&x$
; T
a
0122 kV1kg
o
@
"&st&ll,te-
31. m
1
E C
$N)
E -T
d&x$
/ T
a
0 ; Lm
1
E
N)
MW T
d&x$
; m
2
E C
$w
E -T
d&x$
/T
a
0 ; m
2
E
W"2
o
@
2 kV
9%ere2
W"2
o
@
8
-10
To '&nd
NB
,t T
dexp
-
Met+od 1: qual temperature re*erence plot
T,2le %
ln P
A
ln P
B
Plot ln P

)s ln P
)
and obtain slope. Slope8 * 1 *,N t%us get * 8 slope E *,8
N)
at T
d&x$
Substitute in equation -10.
Met+od %- From t%e 9atson equation

2
1 *
1
8 L-1T+
2
0 1 -1 T+
1
0M

1
8 *
N)
W 6BP2 213
o
@
T
1
8 T
N)P
; 2'3 B
T+
1
8 T
1
1T
'
T+
2
8 -T
d&x$
; 2'30 1 T
'
T
,
1> 8 3.&6' ; T ; -T0
2
N sol)e *or T
'
and subsequently get T+
1
and T+
2
(%en obtain
2
8
N)
Substitute in equation -10 and get t%e )alue o* output %eat
32. (otal output %eat 8 sum o* %eat output in distillate and residue2 kV
33. Dapori5ation e**iciency2 -
V
8 L-m
1
1m
2
0 E -M
w
1M
N)
0M 1 L-P

1-P
T
P

00
W(d
M 8 QQQQQQ
3#. (%ermal e**iciency2 -
T
8 output %eat 1 input %eat E 133 8 QQQQQQ
Gr,)+s to 2e )lotted
1. P

)1s. T and -P
T
/ P
)
0 )1s T
2. ln P
)
)1s. ln P

RESLT-
(%e )apori5ation e**iciency is QQQQQQ.
(%e t%ermal e**iciency is QQQQQQQ.
2#
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