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Experiment Number: 03

Date: September,01, 2023

Name: k.nemalnath reddy

Registration number: 2023003651

Determination of Zinc by EDTA


Method
Objective:
To learn about,

 To understand the behavior of EDTA as chelating agent .

 To know the method of complexometric titration and estimation of metal in materials.

 To know the stability of complexes at particular pH’s.

 Complexometric volumetric titrations with EDTA (ethylenediaminetetraacetic acid) will be


performed. The comprehension and skills learned will be transferable to other laboratory
and workplace situations.

• A primary-standard zinc ion solution will be prepared from primary-standard zinc metal.

• A supplied EDTA solution will be standardized using the primary-standard zinc ion solution.

• The secondary standard EDTA solution will be employed to determine the zinc content of a dietary
supplement.

Introduction:
Determination of the Zinc (Zn+2) by titrating against a standard EDTA solution using Eriochrome
Black-T (EBT) as indicator.

Ethylenediaminetetraacetic Acid (EDTA) : EDTA, the molecular structure of which is shown to the
left below, is the most useful member of a class of compounds called aminopolycarboxylic acids.
EDTA undergoes successive acid dissociations to form a negatively charged ion, shown below to the

right below.

This ion has the ability to “wrap” itself around positive metal ions in water solution. This process is
called chelation or complex formation. The chelation reaction between EDTA and many metal ions
has a very large equilibrium constant. The reaction is always 1 mol of EDTA to 1 mol of metal ion.

Applications of EDTA Chelation (Complexation) ,EDTA has many uses:

• Chemical Analysis of Metals.

• Medical Removal of Heavy Metals in Accidental Poisonings.

• Boiler Water Softening by Chelation.

• Removal of Hard Water Scale by Cleaning Agents.

• Addition to Shampoo to Soften Water.

• Addition to Prepared Food to Prevent Spoilage by Metal Ions.

• Solubilization of Metal Ions in Fertilizers and Vitamin Supplements.

EDTA is not used in residential water softening or home laundry products because it is too expensive
and because it is so effective, it would remove calcium from our bodies if it got into the drinking
water supply.

Reaction of EDTA with Metal Ions :

Except for the alkali metal ions of charge +1, most metal ions in aqueous solution react with EDTA to
form complex ions in solution.

All metal ions react with EDTA in the mol ratio of 1 to 1.

For zinc ions in water:

Zn 2+ (aq) + EDTA4- (aq) -> Zn(EDTA)2- (aq) Kf = 3.2 × 1016

pH Dependence of EDTA Equlibriums (Equilibriums = Equilibria)

Since EDTA is an acid substance with four weak acid dissociations, the reactions with metal ions are
pH dependent. The metal ions that react most strongly with EDTA can be titrated in acidic solution.
Zinc is an example of a metal ion that is titrated in acidic solution.
The metals that react more weakly with EDTA must be titrated in alkaline solution. Calcium and
Magnesium are examples of metal ions that must be titrated in alkaline solution.

To ensure consistent results of titrations, the pH of the solutions must be controlled by using buffer
solutions.

Materials and Equipment:


Chemicals:

Ethylenediaminetetraacetic acid (EDTA), ammonium hydroxide, ammonium chloride, Eriochrome Black T


(EBT), zinc sulphate.

Apparatus: Standard volumetric flask, pipette, burette, conical flask, beakers, funnel and glass rod.

Procedure:
 Standardization of EDTA (~0.01M) Rinse and fill the burette with EDTA solution. Pipette out
10 mL of 0.01M of ZnSO4 solution and add 10 mL of the buffer of pH 10.
 Add 2-3 drops of EBT indicator solution to the flask.
 Titrate the solution from the flask against EDTA solution until the red colour of the solution
changes to blue.
 Repeat the titration to get constant readings.
 Estimation of Zn2+ ions. Rinse and fill the burette with EDTA solution.
 Pipette out 10 mL of Zn2+ ion solution in a conical flask and add 10 mL of the buffer of pH
10.
 Add 2-3 drops of EBT indicator solution to the flask.
 Titrate the solution from the flask against EDTA solution until the red colour of the solution
changes to blue.
 Repeat the titration to get constant readings.

Data and Observations:


The final reading of the burette is noted. Titrations are repeated until 3 or 4 concurrent readings are
obtained. The results are tabulated in Table II.

Table II:

Titration of standard EDTA solution with Unknown zinc solution Molarity of standard solution of
EDTA = Indicator: Eriochrome black-T.

Color change at the end point: Wine red to blue


Sl. No. Volume of Burette Burette Volume of
unknown readings readings EDTA solution
Zinc solution Initial (ml) Final (ml) consumed in
taken in ml ml (V1)
(V2) M
01 10ML 0 8.1 8.1
02 10ML 8.1 15.7 7.6
03 10ML 15.7 23.7 8
AVERAGE:

8.1+7.6+8/3=7.9ML

Calculations and Results:


By the law of equivalence,

M 1V1=M2V2

Molarity of EDTA solution M2 =0.01M

Volume of EDTA solutionV2=7.9L

Molarity of Zinc solution M1=?

Volume of Zinc solutionV1=10ML

 M1 =M2*V2/V1

=0.01*10/7.9

=0.0126M

Report:

The Molarity of Zinc solution, M4 =0.0126M

Equivalent weight of Zinc = atomic weight / 1 = 65.38 / 1 = 65.38 M

Amount of zinc present in 1000 ml of solution = molarity of zinc solution (M1)  equivalent weight of
zinc =0.0126*65.38=0.827 g.

Amount of copper present in the given 100 ml of zinc solution = amount present in 1 liter of the solution
/ 10 =0.827/10 = 0.0827g.

Result:

The amount of zinc present in given unknown sample = 0.0827g.

Discussion: (if any)


The concentration of the Zn solution was determined to be approximately 14 mol/L through the titration
with EDTA. This result is within an acceptable range of the expected concentration.
Conclusion:
The objective of the experiment was successfully achieved by accurately determining the concentration
of the Zn solution. The calculated concentration was 0.0827g, indicating that the experiment was carried
out effectively.

References:
Experiments in Applied Chemistry, S. Rattan, S. K Kataria and Sons.

Vogel’s textbook of quantitative chemical analysis, J. Mendham, R. C. Denney, J. D. Barns, M.


Thomas, B. Sivasankar, Pearson India Education, 6th Edition.

The student remarks on experiment:


Sources of Error:

1. regular water instead of distilled water.


2. No Care is taken while preparing cement solution .
3. There may be any leakage from burette.
4. Before using any solution, not shaking it properly.

Precautions:

 The fumes from the NH3/NH4Cl buffer at pH 10 are toxic, corrosive, and irritating.
 Wash hands thoroughly before leaving the lab.
 Eriochrome black-T is a dye stuff and avoid direct contact since it cause eye irritation and
skin irritation.
 Don’t add excess amount indicator to avoid error.
Remarks:

 What is the theoretical endpoint of a complexometric titration?


 How complexation stabilize the metal ions?
 What is the importance of pH in complexometric titration?
 List any two applications of EDTA titration.
 How a mixture of Ca and Mg can be determined volumetrically?

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