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KWAME NKRUMAH UNIVERSITY OF SCIENCE

AND TECHNOLOGY

COLLEGE OF ENGINEERING
DEPARTMENT OF CHEMICAL ENGINEERING

TITLE: ESTIMATION OF CALCIUM IN A


SAMPLE SOLUTION WITH EDTA
NAME:

KWAKYI KOFI BOSOMPEM

COURSE:

BSC. CHEMICAL ENGINEERING

YEAR:

second

EXPERIMENT NO. : A.1.2.2.


I.D. NO:

9664813

DEMONSTRATOR:

EMMANUEL AGYEMAN DUAH

DATE:

25th February 2015.

POST LAB

1. What kind of water hardness can EDTA eliminate?


2. Why the adddition of a buffer solution for the estimation of calcium in a
sample solution with EDTA?
3. Explain the chemistry before and at the endpoint of the titration.

solution
1. EDTA eliminates temporal hardness of water.

2. EDTA solutions are usually buffered in a region to ensure that protonation


reactions do not compete with the complexation reaction. And also In
order to obtain good results

3. Before the endpoint of the titration, the solution is purple because of the
excess metal ion. As the EDTA titrant complexes more and more metal, the
above equilibrium shifts to the left. At the endpoint the solution turns blue.

AIMS AND OBJECTIVES

To know what an EDTA is, its functions and its structure.

To acquire more knowledge using the analytical balance to weigh


substances.
To estimate the amount of calcium in calcium carbonate with EDTA.

SAFETY PRECAUTIONS

Safety glasses and aprons must be worn at all times in the lab.
Solutions, other chemicals and experimental apparatus should be handled
with care since spillage and breakages can cause injuries.

INTRODUCTION/THEORY
Many metals form complexes which contain appropriate ligands EDTA is one
such reagent which forms complexes with metals. In the form of its disodium
salt, it is used to eliminate ca2+ and mg+4 ions.
EDTA reacts with a metal in a 1:1 ratio to form a hexadentate chelate. EDTA
contains six sites that can be protonated. Since EDTA itself is quite insoluble in
water, the disodium salt is normally used to make EDTA solutions. To form the
strongest complexes, EDTA solutions are usually buffered in a region that ensures
that protonation reactions do not compete with the complexation reaction.
Chelates are very stable andmostare soluble.
M+n + Y-4 MYn-4
The formation of chelates due to complexometry is used to determine the
amount of substance. Water hardness on one thing that come be determined.
Water hardness id defined as a measure of the capacity of water to precipitate
soap. Soap is precipitated chiefly by the calcium and magnesium ions
present.the major ions responsible for water hardness are therefore calcium and
magnesiumwith lesseramounts of iron and other metals.

EXPERIMENTAL APPARATUS AND CHEMICAL


Equipment
250ml volumetric flask
Burette
Pipette
Retort stand
Conical flask
Measuring cylinder
Analytical balance
Beaker

Chemic
als
CaCO3
HCl
EDTA
Calcium solution
Solochrome Black T indicator

PROCEDURE
2.5g of the CaCO3 was weighed and transferred into a beaker. Dilute HCl was
added in drops till effervescence seized and the solution was transferred into a
250ml volumetrick flask, dilute water was then added to the250ml mark.
10ml of the prepared calcium solution was pipetted into the 250ml conical flask.
20ml distilled water was added and then 2ml buffer solution and 5 to 6 drops of
the indicator solution was added. EDTA was added from the burette drop wise till
the purple colour of the solution changed to permanent blue. The volume was
recorded.
The end point of the titration is recorded. The titration was repeated to get
concordant values.
m(CaCO 3)=2.5g

TABLE OF RESULTS
Burette Readings/cm3

Final reading

13.10

13.20

13.10

Initial reading

0.00

0.00

0.00

Titre values

13.10

13.20

13.10

Average titre =

(13.10+13.20+13.10)
3

= 13.13cm3

CALCULATIONS
Titration reaction: H4Y + Ca2+

CaH2Y +2H+

Mole ratio of H4Y to Ca2+= 1:1


H4Y= 0.1M
If 1000ml=0.1

(13.16 0.1)
1000

n(Ca2+) in 25ml of the solution=

n(Ca2+) in 250ml of the solution =

250 0.001131
25

= 0.01313 mol

1.313 10-3

Number of moles =

MASS
MOLAR MASS

m(Ca 2+) = 0.01313 40


= 0.525g
Therefore the percentage of Ca in 2.5g of CaCO 3 = (0.525/2.5) x 100% =
21.01% 21%

DISCUSSION
From the experiment, the values of the titration was 13.10, 13.20 and 13.10 at
the end point, indicating that they were very consistent.

The structure of EDTA


HOOC-H2C

CH2-COOH
N-CH2- CH2-N

HOOC-H2C

CH2-COOH

Since EDTA forms very strong complexes with most metal ions with a charge
greater than +2, procedures designed to "mask" or complex impurity ions are
often used. In this experiment, however, relatively pure calcium carbonate
unknowns are used so that masking reagents are not needed. The overall
procedure to be used involves the standardization of an EDTA solution by
titration with a known amount of calcium followed by using the calibrated
solution to determine an unknown amount of calcium.
If the EDTA molecule is represented as H 4Y, where the four acidic hydrogen
atoms are those at the ends of the molecule, then EDTA dissolved at pH l0 is
approximately half in the form of HY3- and half in the form of Y4-. The two ends of
EDTA are replaced with the calcium ion and hydrogen ion is released into
solution, making the solution slightly acidic. The complexation reaction of EDTA
with Ca2+ can therefore be represented in either of the following ways, where M 2+
represents the metal ion.

EXPERIMENTAL PRECAUTION

The weighing balance was set to the zero mark before weighing the
amount of CaCO3.
Accurate volume of H2O, Buffer solution and indicator was used.
All readings recorded were taken below the meniscus of the liquid.
All apparatus were washed and rinsed with distilled water before use.
Accurate and appropriate amount of indicator was added.

CONCLUSION
From the experiment, it can be concluded that, the mass of Calcium in the
solution was 0.525g. This implies that EDTA is used in the determination of
Calcium and the experiment was successful.

REFFERENCES

KNUST laboratory Manual, Department of Chemistry, page 43.

Essential chemistry by Raymond Chang (page 863), 4 th edition.

Wikipedia