Preparation of column:

1. Put a piece of glass wool or cotton on the bottom of a small burette.

2. Weight out accurately about 1g of the anion exchange resin (R-OH)
on a sensitive balance, and transfer quantitatively to the burette
(after removing the fine particle by putting the resin in a beaker
with D.W by decantation) and sufficient D.W to cover the resin, no
air bubbles should be present.
25ml D.W.
1g R-OH resin
removing the fine particle
By decantation
Decantation
Sensitive balance
3. Put another piece of glass wool on the top of the surface of the resin inside the burette.

Regeneration
Regeneration • 5ml 1M NaOH
• wash the resin by D.W.
By 5ml 1M NaOH (to remove excess NaOH)
until litmus paper color don’t
convert to blue
• F.R =1-2ml/min
Glass wool or cotton

Litmus paper

4. Regeneration the resin by 5ml 1M NaOH with (F.R = 1-2ml/min) and wash the
resin with D.W to remove excess NaOH until the effluent become neutral (test
effluent by litmus Paper until its color don’t convert to blue).
Procedure:
1. Prepare 50ml of 1M NaCl solution in a volumetric flask, transfer it to a (50ml
separation funnel).

transfer 50ml 1M NaCl

50 ml volumetric flask 50 ml separation funnel

2. Put the separation funnel on the top of the column.

R-OH

Stand and clamp

 50ml 1M NaCl 3. Pass the NaCl solution
• flow rate constant (1-2ml/min)

V(ml) HCl
R-OH
Complete by Std. 0.05N HCl
D.W.

4., 5. Collect all the effluent

7. Take 25ml 3 drops
(each 2ml in a cylinder )
Ph.Ph
Until color litmus paper indicator
not change to blue 6. Combine all the
effluent in 100ml
volumetric flask,
8. Find the capacity of the anion exchange resin
Calculation: Exchanger process:

Wt.(g) of Resin R-OH = 1g

V(ml) – OH liberated V(ml) HCl (0.05N)

25 V1 from burette
25 V2 from burette
Vav = (V1+V2)/2
V(ml) HCl
At the end point Std. 0.05N HCl
No. of meq. – OH liberated in 25ml = No. of meq. HCl
= (N × Vav) HCl

–
100
No. of meq. OH liberated in 100ml = (N × Vav) HCl × 3 drops Ph.Ph
25
indicator
No. of meq. – OH liberated
Capacity of R-OH (meq/g)=
Wt.(g) Resin
Experiment 7:

Procedure:
1. 1g Anion exchange resin
Cl- (R-OH) Br-
2. Regeneration
• Add 5ml 1M NaOH
stir for 5 min
Label Cl- Label Br-
filtration • Wash by D.W to remove all NaOH
• Test by Litmus Paper filtration
• Color doesn’t convert to blue.

×
 3. Prepare
50ml 0.01M NaCl
50ml of 0.01M KBr
Cl- Br-
4. Wait 20-30 min
• stir time to time

5. Filtration 5. Filtration
 Complete by D.W.

V(ml) AgNO3=O V(ml) HCl V(ml) AgNO3=O

V(ml) HCl
Std. 0.05N AgNO3 Std. 0.05N HCl Std. 0.05N AgNO3
Std. 0.05N HCl

3drops M.red 3drops M.red

indicator 0.5ml K2CrO4 indicator 0.5ml K2CrO4
indicator indicator
Yellow Red
Yellow Red Yellow Brown Yellow Brown
Blank titration

V(ml) AgNO3=E
Std. 0.05N AgNO3

25ml D.W.

0.5ml K2CrO4 indicator

Yellow Brown
Experiment 7:

For Cl-
V(ml) Cl – remain in solution V(ml) AgNO3 (0.05N) NaCl = 0.01N
25 V1 from burette V(ml) = 50ml
25 V2 from burette
Vav = (V1+V2)/2 = O

V(ml) –OH liberated V(ml) std. HCl (0.05N)

25 V1 from burette
25 V2 from burette
Vav = (V1+V2)/2

Wt.(g) of Resin R-OH = 1g V(ml) AgNO3 for blank = E

For Br-
V(ml) Br – remain in solution V(ml) AgNO3 (0.05N)
KBr = 0.01N
25 V1 from burette V(ml) = 50ml
25 V2 from burette
Vav = (V1+V2)/2 = O

V(ml) –OH liberated V(ml) std. HCl (0.05N)

25 V1 from burette
25 V2 from burette
Vav = (V1+V2)/2

For Cl-

Total m.eq.wt (R—OH) = Capacity * wt. Resin = (meq.wt / g) * wt.(g) Resin

Result of Exp. (No.1)
No. of meq.wt [OH] librated = meq.wt HCl
(in solution) in 25ml

100
Total no. of meq.wt [OH] librated = (N × Vml)HCl × [OH]s
25
(in solution) in 100ml

Total no. of meq.wt (R-OH) – meq.wt [OH] librated = meq.wt (R-OH)

(in solution) in 100ml (remain on resin)

100
Total meq.wt (R-OH) - (N × Vml)HCl × = meq.wt (R-OH) [R-OH]r
25
(remain on resin)

Total no. of meq.wt NaCl or Cl = (N × V) NaCl = 0.01 × 50 = 0.5 meq.wt

No. of meq.wt (Cl) NaCl or remained = meq.wt AgNO3 = NAgNO3 × (O-E)
100
No.of meq.wt (Cl) remained in total soln. = NAgNO3 × (O-E) × [Cl]s
25

Total no meq.wt [NaCl] or [Cl] – Total meq.wt [Cl] remained = meq.wt (R-Cl ) [R-Cl]r
Cl exchanged
 Amount of solute (Cl) on resin 𝑅−𝐶𝑙 𝑟
1. Distribution constant KdCl = = or
Wt.(g) Resin Wt.(g) Resin
𝐶𝑙 𝑟
Wt.(g) Resin
By the same way find KdBr

KdCl KdBr
2. Separation factor (α) :- α = or
KdBr KdCl
If α > 1.2 or α < 0.8 the separation of mixture [Cl- + Br-] is possible by the resin.
3. Selectivity coefficient E:-

Cl [Cl−]on resin [OH] soln. [Cl−]r [OH]s [ R−Cl]r [OH]s

EOH = or or
[OH]on resin [Cl−]remain in soln. [OH]r [Cl−]r [R−OH]r [Cl−]s
𝐁𝐫
By the same way find 𝐄𝐎𝐇
 Preparation of column:
1. Put a piece of glass wool or cotton on the bottom of a small burette.
2. Weight out accurately about 1g of the anion exchange resin (R-OH) on a
sensitive balance, and transfer quantitatively to the burette (after removing
the fine particle by putting the resin in a beaker with D.W by decantation)
and sufficient D.W to cover the resin, no air bubbles should be present.

25ml D.W.
1g R-OH resin
removing the fine particle
By decantation
Decantation
Sensitive balance
3. Put another piece of glass wool on the top of the surface of the resin inside the burette.

Regeneration
Regeneration • 5ml 1M NaOH
• wash the resin by D.W.
By 5ml 1M NaOH (to remove excess NaOH)
until litmus paper color don’t
convert to blue
• F.R =1-2ml/min
Glass wool or cotton

Litmus paper

4. Regeneration the resin by 5ml 1M NaOH with (F.R = 1-2ml/min) and wash the
resin with D.W to remove excess NaOH until the effluent become neutral (test
effluent by litmus Paper until its color don’t convert to blue).
Procedure: Elution Cl-
3. Added 5ml 0.3M KNO3
1. 0.05g NaCl Transfer to Flow rate must be constant
Dissolve
0.1g KBr) the top of the (F.R =1-2ml/min)
column
2ml D.W.

R-Cl
R-Br

2. Blank titration

• Continuous collection
V(ml) AgNO3=E
5ml solution of the solution and titration
Std. 0.02N AgNO3
Contain Cl- until O≈E
V(ml) AgNO3=O
Std. 0.02N AgNO3
5ml 0.3M KNO3
5ml solution
or 0.3M NaNO3
Contain Cl-
0.5ml K2CrO4 indicator
0.5ml K2CrO4
indicator
Yellow Brown
Yellow Brown
 Elution Br-
R-Br 3. Added 5ml 0.6M KNO3
Flow rate must be constant
(F.R =1-2ml/min)

6. Blank titration

• Continuous collection
V(ml) AgNO3=E
5ml solution of the solution and titration
Std. 0.02N AgNO3
Contain Br- until O≈E
V(ml) AgNO3=O
Std. 0.02N AgNO3
25ml 0.6M KNO3
or 0.6M NaNO3 5ml solution
Contain Br-
0.5ml K2CrO4 indicator
0.5ml K2CrO4
indicator
Yellow Brown
Yellow Brown
Calculation:
 Experiment 9:

Preparation of column:
1. Put a piece of glass wool or cotton on the bottom of a small burette.
2. Weight out accurately about 1g of the cation exchange resin (R-H)
on a sensitive balance, and transfer quantitatively to the burette
(after removing the fine particle by putting the resin in a beaker
with D.W by decantation) and sufficient D.W to cover the resin, no
air bubbles should be present.

25ml D.W.
15g R-H resin
removing the fine particle
By decantation
Decantation
Sensitive balance
3. Put another piece of glass wool on the top of the surface of the resin inside the burette.

Regeneration
• 5ml 6M HCl
4. Regeneration • wash the resin by D.W.
(to remove excess HCl)
until test the effluent by
AgNO3 no ppt. or turbidity
appear
Glass wool or cotton • F.R =5ml/min

4. Regeneration the resin by 5ml 6M HCl with (F.R = 5ml/min) and wash the resin
with D.W to remove excess HCl until test the effluent by adding AgNO3 there is no
ppt. or turbidity appear or test by acid- base indicator.
 Procedure:
2. Pass 3 portions
1. 10ml mixture (H+, Na+, Mg2+, Zn2+) (25ml D.W)
flow rate 5ml / min

V1(ml) Std. NaOH

10ml Solution contain

3. Collection all effluents H+
Take 3 drops
Solution contain H+ bromocresol green
complete by D.W. to 10ml
100ml Volumetric flask
Yellow Blue
Determination of mixture ions (H+, Na+, Mg2+, Zn2+)
V(ml) H+ liberated V(ml) std. NaOH
10 ml V1
(H+, Na+, Mg+, Zn) mixture + R-H R-H+, R-Na+, R-Mg2+, R-Zn2++ H+ liberated

no. of mmole (H+) liberated = no. of mmole NaOH= total no. of mmole ions
𝟏𝟎𝟎
Total no. of mmole ions (H+, Na+, Mg2+, Zn2+) = (N * V1)NaOH x 𝟏𝟎
4. Determination H+ in mixture solution V2(ml) Std. NaOH

V(ml) mixture ions V(ml) std. NaOH

10 ml V2

4. 10ml mixture solution

75ml D.W
3 drops
bromocresol green
Yellow Blue

At the end point

no. of mmole (H+) in mix.= mmole NaOH = (N * V2)NaOH
Total no. mmole of ions – no. mmole of (H+) in mix.= no. mmole of (Na+, Mg2+, Zn2+)
(NNaOH* V1) - (NNaOH* V2) = no. of mmole (Na+, Mg2+, Zn2+)
5. Determination Mg2+ , Zn2+ in mixture solution V3(ml) Std. EDTA

V(ml) mixture ions V(ml) EDTA

10 ml V3

5. 10ml mixture solution

V2 (ml) NaOH
2ml buffer PH 10
0.1g EBT indicator

Violet Blue

At the end point

No. of mmole (Mg2+, Zn2+) = No. of mmole EDTA
No. of mmole (Mg2+, Zn2+) = (M * V3) EDTA
From step 4
No. mmole of (Na+, Mg2+, Zn2+) - mmole ( Mg2+ , Zn2+) = mmole of (Na+)
6. Determination Mg2+ in mixture solution 7. V4(ml) Std. EDTA

V(ml) mixture ions V(ml) EDTA

10 ml V4

6. 10ml mixture solution

V2 (ml) NaOH
0.5g KCN
2ml buffer PH 10
0.1g EBT indicator

Violet Blue

At the end point

no. of mmole (Mg2+) = no. of mmole EDTA = (M * V4) EDTA
From steps 5,6
no. of mmole (Mg2+, Zn2+) Result of step5 – no. of mmole (Mg2+) Result of step6
= no. of mmole (Zn2+) no. of mmole (Zn2+) = (M * V3)EDTA - (M * V4)EDTA
Experiment 12:

Cotton
1. 5ml mixture (0.05M of each KMnO4 and K2Cr2O7) or Wool
5g Al2O3
Elution KMnO4

Passing D.W. until pink colour disappear

V(ml) Std. Fe2+

K2Cr2O7

KMnO4

25ml solution
Complete Take 10ml 0.5M H2SO4
By D.W 25ml

Effluent solution 100ml Vol. flask

KMnO4
Pink colourless
 Elution K2Cr2O7

Passing 0.25M H2SO4 until orange Zone disappear

V(ml) Std. Fe2+

K2Cr2O7

25ml solution
Complete Take 3 drops DPA indicator
By D.W 25ml

Effluent solution 100ml Vol. flask

K2Cr2O7
yellow green violet
Calculation:
1. Determination of KMnO4 by titration with std. Fe2+
V(ml) KMnO4 V(ml) Std. Fe2+
25ml V1 from burette
25ml V2 from burette
Vav = (V1+V2)/2

No. mmole KMnO4 1

=
No. mmole Fe2+ 5

1
No. mmole KMnO4= x No. mmole Fe2+
5

W mg KMnO4in 25m1 1
mg = x (M x Vav) Fe2+
M.wt.
mmol
KMnO 4
5
 1 mg
W(mg) KMnO4 in 25m1= x (M x Vav) Fe2+ x M. wt. KMnO4
5 mmol

1 100
W(g) KMnO4 in 100m1 (Collect) = x (M x Vav) Fe2+ x 158 x x 10−3
5 25

M x M. wt. KMnO4 x V(𝑚𝑙) 0.05 x 158 𝑥 5

W g KMnO4 in mixture = =
1000 1000

W g KMnO4 collect
% Recovery for KMnO4 = W x 100
g KMnO4 in mixture

2. Determination of K2Cr2O7 by titration with std. Fe2+

V(ml) K2Cr2O7 V(ml) std. Fe2+

10 V1 from burette
10 V2 from burette
Vav = (V1+V2)/2
No. mmole K2Cr2O7 1
=
No. mmole Fe2+ 6

1
No. mmole K2Cr2O7 = x No. mmole Fe2+
6

W mg K2Cr2O7 in 25m1 1
mg = x (M x Vav) Fe2+
M.Wt.
mmol
K Cr O
2 2 7
6

1 mg
W(mg) K2Cr2O7 in 25m1= x (M x Vav) Fe2+ x M. wt. K2Cr2O7
6 mmol

1 100
W(g) K2Cr2O7 in 100m1 (Collect) = x (M x Vav) Fe2+ x 294 x x 10−3
6 25

M x M.wt. K2Cr2O7 x V(𝑚𝑙) 0.05 x 294 𝑥 5

W g K2Cr2O7 in mixture = =
1000 1000

W g
2 K Cr O
2 7 collect
% Recovery for K2Cr2O7 = W g K Cr x 100
2 2O7 in mixture