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COLUMN CHROMATOGRAPHY

SMK Negeri 13 Bandung


R+OH- + X- === R+X- + OH-
n R-H+ + Mn+ === (R)n-Mn+ + n H+
Objective
After this session the students are
expected to be able to conduct the
analysis of chemical substance using
the ion exchanger resin.
ION EXCHANGER RESIN


Definition : ion exchange from
the same charge ions between the
solution and the insoluble solid

Condition
The solid substance to exchange
should have the same ion with the ion
in solution
Molecular structure of solid has an
opened structure and permeable
(easy to be penetrated) so the solute
is easy come and out. Exchanging
process will be past and efficient

ION EXCHANGER RESIN
The solid substance is stationary
phase and the solution is mobile
phase.
Solid ion exchanger is made of
polymer polystirene cross-linked with
divinyl benzee. Polymer with cross-
linking called resin. It has free phenyl
group easy to react with ionic
functional group (addition)
Resin used in analysis to separate
inorganic ions (cation and anion)
Ptroperties of Ion Exchanger Resin
1. Insoluble in water but has an ability to
absorbp water molecule in it structure.
2. Has a high molecular relative mass (High
Mr).
3. Resistant to chemical substance (Acid,
base, organic solvent)
4. When an ionic solution flow in to resin, it
will release an ion and at the same time it
will capture an ion of the solution.
5. Ion exchange carry out on the same type
ion (cation with cation, anion with anion).

4 types of ion exchanger resin
1. Strong acid cation exchanger. The
exchanger functional group is sulfonic
acid.
2. Weak acid cation exchanger. The
exchanger functional group is carboxilic
acid.
3. Strong base anion exchanger. The
exchanger functional group is quarterner
ammonium ion.
4. Weak base anion exchanger. The
exchanger functional group is anion group.
(Cation Exchanger Resin)
A column filled by acid / R-H
to exchange cations in
solution with H
+
ion in the
resin.
R
z
H + C
+
R
z
C
+ H
+
C
+
could be : Na
+
, K
+
, Ca
2+
,
Mg
2+
, etc.
Cation Exchanger Resin
In weak acid exchanging type, H is
carboxilic acid that only partly
ionized. The reaction is:

nR
z
CO
2
H
+
+ M
n+
(R
z
CO
2
)
n
M + nH
+


In strong acid exchanging type, H is
sulfonic acid group. It is strong acid
like sulfuric acid. The reaction is.

nR
z
SO
3-
+ M
n+
(R
z
SO
3
)
n
M + nH
+


(Cation Exchanger Resin)
(Anion Exchanger Resin)
A column filled by base / R-
OH to exchange anions in
solution with OH
-
ion in the
resin.
R
Z
OH + A
-
R
Z
A + OH
-
A
-
could be : Cl
-
, SO
4
2-
, NO
3
-
, etc.
(Anion Exchanger Resin)
In strong base anion exchanger, the
reaction is :

n
R
z
NR
3
+
OH
-
+ A
n-
(R
z
NR
3
)nA +
n
OH
-

Ion Exchanger Selectivity
There are 2 factors influence the
selectivity :
The exchanged ions properties
The ion exchanger properties.
Exchanged ions properties:
At room temperature and low
concentration, ion with higher
charge will tightly held by resin.
Ex : Al
3+
> Ca
2+
> Na
+
In the same condition for the same
charge ion :
+1 ion
Lower the size of ion, stronger the resin hold the ion.
Ex : Li
+
< H
+
< Na
+
< NH
4+
< K
+
+2 ion
Resin absorption determinated by the ion size and
dissosiation of salt .
Ex : Cd
2+
< Ba
2+
< Mn
2+
< Mg
2+
= Zn
2+
< Cu
2+
< Co
2+

Exchanged ions properties:
In strong base ion exchanger -1
anionhas the equivalent absorption
selectivity with the +1 cation. (Lower
the size of ion, stronger the resin hold
the ion)
Ex : F
-
< HCO
3-
< Cl
-
< HSO
3-
< OH
-
< Br
-
<
NO
3-
< I
-


In dilute solution -X anion (X>1)
absorbed stronger than the -1 anion.


When the charge of cations to be
exchanged is not same. Ion activity
with the higher charge is higher
when the concentration of higher
charge ion is lower.
Example :
M
+2
in solution and M
+1
in resin will
effectively exchanged at low
concentration
M
+1
in solution and M
+2
in resin will
effectively exchanged at high
concentration.
Ion exchanger properties
Quantitatively, afinity of ion exchanger resin
to the exchanged ions terms as distribution
coefficient (D):
sama yang pelat pada larutan dalam sampel Kuantitas
entu pelat tert pada resin dalam sampel Kuantitas
D
Complexing agent

Complexing agent is anions like Cl
-
, Br
-
and I
-
which
have ligand nature. The complexion is influenced by
pH value.
Many metals could be separated in anion exchanger
column after transformed to anion by complexing
agent.
Metal separation in anion exchanger column carry
out by addition of high concentration acid to
transform metal ion to be complex anion.
Example
Concentrated HCL forms complex anion with most
metal except alkali and earth alkali metal.
Al(III), Ni(II), dan Cr(III) form complex anion with
Cl
-
.
Almost all complex anion of metal absorbed by
quarternar ammonium resin.
Resin Regeneration
Amount of cation and anion to be exchanged
by resin depends on the resin capacity.
When resin absorb amount of ion more than
its capacity, resin is exhausted. It should be
regenerated.
Regeneration of anion exchanger resin :
Acid : HCl, H
2
SO
4
.
Reaction : Rz C + H
+
Rz H + C
+
Regeneration of cation exchanger resin :
Base : NaOH.
Reaction : Rz A + OH
-
Rz OH + A
-
Resin Column
a
.