Date:

Expt. No.
and its
Water Purification Hardness Estimnation by EDTA method
Experiment Removal using lon-exchange Resin
Hardness of water is due to the presence of dissolved calcium and
hardness
magnesium salts in water. EDTAforms stable complex with
Problem definition
causing salts and is used in the removal of scale and sludge forming
impurities in industrial boilers.
EDTA-metal
EBT indicator-Metal ion complex is weaker compared to
red (EBT
Methodology ion complex. The end point is the color change from wine
Metal ion complex) to steel blue (free EBT indicator).
Estimation of Calcium hardness (in ppm) in the given unknown
Solution
sample. Understanding the water softening using ion-exchange resins.
Students will learn to
Student learning a) perform complexometric titration
outcomes b) understand the efficiency of ion-exchange resins using in water
purifiers

Principle:
Ehtylenediaminetetraacetic acid (EDTA), forms complexes with a large number of cations
determine
including Ca* and Mg depend ing upon pH of solution. Hence, it is possible to
form of its sodium salt
the total hardness of water using EDTA solution. EDTA in the
because
(H2Y) is commonly used in complexometric titration for estimation of metal ion
sites (the four
pure EDTA (H4Y) is sparingly soluble in water. EDTA has six binding
The resulting
carboxylate groupsand the two amino groups) providing six pairs of electrons.
metal ion, is
metal-ligand complex, in which EDTA forms a cage-like structure around the
The Hay?
very stable at specific pH. AIlmetal-EDTA complexes have a 1:1 stoichiometry.
form complexes with metal ions as follows.
M+ H,Y² ’ MY?+ 2H (1)
Where, M is Ca* and Mg present in water. Reaction (1) can be carried out quantitatively
complexX with
at pH 10 using, Eriochrome Black T(EBT) s indicator. EBT forms a wine-red
M2* ions which is relatively less stable than the M"-EDTA complex. On titration, EDTA
first reacts with free M²* ions and then with the metal-EBT indicator complex. The latter
gives a colour change from wine-red to steel blue at the equivalence point.

Removal of hardnes using ion exchange resins (ER): lon exchange is a reversible
process. When hard water is passed through cation ion-exchange resins packed in a narrow
column, Ca and Mg+ cations in hard water are exchanged with Nat or H+ ions in the

2
 column. A
resins. The exhausted resins are regenerated by passing 10% dil. HCIthrough the
typical example of application is preparation of high-purity water for power engineering,
electronic and nuclear industries and in household water purifiers.

Soft wratrt out lad wster tn

Caldun and
Hard water pours Treated mOsiun ions
to a treatment water to
tank home Bsckrash out
-Hand water
flows around
Reua echurgo
plastic besds 1Na eplace C
Brine ank COvered with Hanl waner in
sodium kons.

CO0Na CO0 N c
Sodium swaps coON cOONa
places with the
calcium d R-Q00A N R-COO
Plastic magnes
Deds CO0
Detai!
N N
-CO0 coo c
COO Na
2 Na
Sodum ions
Brine is
Carsrdge ABel eieh reún
C cpse 2 Na
Dran
Resto dishargod

Requirements
Reagents and solutions: Standard hard water (I mg/mL of CaCO3 equivalents), 0.01 N
EDTA solution, EBT indicator, hard water sample, NH3-NH4Cl buffer solution and ion
exchange resin.
Apparatus: Burette, pipette, conical flask, standard flask burette stand and IER column.

Procedure
Titration-I: Standardization of EDTA
Pipette out 20 mL of the standard hard water containing Img/mL of CaCO3 (1000 ppm) into
a clean conical flask. Add one test tube full of ammonia buffer (NHOH- NHC) so lution
indicator
to maintain the pH around 10. Add three drops of Eriochrome Black - T (EBT)
and titrate it against the given EDTA solution taken in the burette. The end point is change
of colour from wine red to steel blue. Repeat the titration for concordant titer values. Let
V' be the volume of EDTAconsumed.

S. Volume of standard hard water Burette reading (mL) Volume of EDTA

No. (mL) Initial Final (V1, mL)
1
20m2 2-2 ml 21"2 me
2
20nl 196ml 196nml

Concordant titer value

q:3n

3
Caleulation:
20 mL of given hard water consumes Vi mL of EDTA
20 mg of CaCO3 requires V1 mL of EDTA for complexation
:.1mL of EDTA requires = 20/V1 mg CaCO; for complexation

This relation will be used in other two titrations

Titration-II: Estimation of total hardness of hard water sample

a clean conical flask. Add one test
Pipette out 20 mL of the given sample of hard water into
solution and three drops of Eriochrome
tube full of ammonia buffer (NHOH NH,CI)
ized EDTA solution taken in
Black-T (EBT) indicator. Titrate this mixture against standard
wine red to steel blue. Repeat the
the burette. The end point is the change of color from
consumed.
titration for concordant titer value, Let V,' be the volume of EDTA
Volume of EDTA
S. Volume of sample hard water (mL) Burette reading (mL)
Initial Final (V2, mL)
No.
1 15:4 me
20 ml 15:Lml
2
20 ml 15:Lml
3
Concordant titer value 15-25ml

Calculation:
From Titration 1, we have the following relation:
complexation
.. 1mL of EDTA requires =20/V1 mg CaCO; for
From Titration 2.,
V2 mL of EDTA,
20 mL of sample hard water consumes =
=V2x 20/Vi mg of CaCO; eq.
20/VËx 1000/20
.:.1000mL of hardwater sample consumes = V2 x
= Va/V1x1000 ppm
Total hardness of the water sample= "X ppm

Titration-3: Removal of hardness using ion exchange method

clean funnel on top of the
Arrange the ion exchange co lumn on to a burette stand and place a
completion of
column. Pour the hard water sample (around 40 to 50 mL) remaining after the
clean beaker
Titration- 2 through the funnel and into the ion exchange column. Place a
a period of
under the column and collect the waterpassing through the column over
1Ominutes, Adjust the valve of the column to match the duration of outflow.
Erom the water collected through the column, pipette out 20 mL into a clean conical flask
of EDTA
and repeat the EDTA titration as carried out above. Note down the volume
consumed as V;.

4
Calculation:
From Titration 1, we have the following relation:
i. 1mL of EDTA requires = 20/Vi mg CaCO, for complexation
From this relation, it can be seen that
20 mL of water sample after softening through the column consumes = V3 m of EDTA.
= V3x 20Ni mg of CaCO; eq.
:. 1000 mL of water sample after softening through the column consumes =
= V3 x 20/V1x 1000/20
=V/V1x1000 ppm
.:. Residual hardness of the water sample =Y" ppm

Burette reading (mL) Volume of EDTA

S. Volume of sample hard water (mL)
(V3, mL)
No. Initial Finak
1
20
2
3
Concordant titer value

Result:
Total hardness of the water sample=743 (X) ppm
Residual hardness in the water sample S:l8 (Y) ppm
Keg no: 23 BASoo 7
Hardness removed through the column = 23:42 (X-Y) ppm