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SMJC 2701

ANALYTICAL LABORATORY

NAME : NURSHAFIKA BINTI SHAHLI


PARTNER NAME : 1. RASHIATUN BINTI MOHD RASID
2. NURUL RAQIBAH BINTI RIDWAN
3.ESTHER GANIT PENGIRAN
4. CLERA A/P PETER JOHN
5.JAALYNEE A/P KANNIAPPAN

SECTION : 02

EXPERIMENT NO : 2

EXPERIMENT TITLE : COMPLEXOMETRIC TITRATION

DATE OF EXPERIMENT : 3 APRIL 2019

LECTURE’S NAME : DR KAMYAR SHAMELI

DEMO’S NAME : 1. MOSTAFA YUSEFI

2.NUR AFINI ISMAIL


1.0 EXPERIMENT NO
2

2.0 EXPERIMENT TITLE


COMPLEXOMETRIC TITRATION

3.0 OBJECTIVES
After doing the experiment, the students are expected to able to:
1. Student should know to define a complexometric titration.
2. Describe the reaction between a metal cation and EDTA.
3.Calculate the concentration the unknown solution given the titration data .

4.0 INTRODUCTION
In this experiment you will use ethylenediaminetetraaectic acid (EDTA) to determine metals in
aqueous solution by complexation titration. EDTA is a chelating agent that binds to metals through four
carboxylic acids. Its formation constant for complexation is different for each metal, and because the
ligands are acids, the formation constants are also strongly dependent on pH. Metals always bind more
strongly as pH increases because acidic hydrogens are removed from the EDTA. By controlling pH you
can favor complexation of one metal over another. EDTA is colorless whether or not it is bound to a
metal ion. Endpoints for complexation titrations can be observed using metal ion indicators such as
Eriochrome Black T. This compound is wine red when complexed with metal ions, and blue in the free
form. Addition of the indicator to a solution containing metal ions turns the solution red due to metal ion
binding. EDTA binds metals more strongly than the indicators, so when all of the metal ions are bound to
EDTA, the indicator is left in its free form, and the solution turns blue.

Complexometric titrations with EDTA have been reported for the analysis of nearly all metal
ions. Because EDTA has four acidic protons, the formation of metal-ion/EDTA complexes is dependent
upon the pH. For the titration of Zn2+, one must buffer the solution to a pH of 10 so that complex
formation will be quantitative. The reaction of Zn2+ with EDTA may be expressed as: Zn2+ +
(EDTA)4- → [Zn(EDTA)]2-
This reaction can be used to determine the concentration of zinc ion by using an EDTA standard
solution and an indicator which can form a colored complex with Zn2+. The following two factors are
important for determination of the concentration:
i) The indicator used must form a complex with zinc (much more slowly) compared to the EDTA. Zn2+
indicator complex should only form after all the EDTA has reacted with the Zn2+ cation.

ii) Zn2+ indicator complex must have a different colour from the indicator. “Eriochrome Black T” (EBT)
indicator, fulfill all the requirements mentioned earlier and can be used for this purpose. This method of
determination is the simplest way to determine the concentration of the metal because 1 mol of EDTA
usually reacts with 1 mol of metal.

5.0 PROCEDURE

APPARATUS

1.250 cm3 volumetric flask.

2.250 cm3 conical flask.

3. Burette.

4. Retort stand.

MATERIAL

1. EDTA salt (disodium hydrate).

2. EBT indicator.

3. Buffer solution (ammonium chloride in ammonia).

4. Zn2+ solution.

5. Magnesium complex solution.


a. Standardization of EDTA solution

1. The burette was rinsed with small amount of the dilute EDTA solution and drained it,then the burette was filled
to mark.

2. 12.5 cm3 of the calcium carbonate solution was pipette given into the 250 cm3 Erlenmeyer flask.

3. 50 cm3 was diluted with distilled water

4. 1 cm3 of magnesium complex solution was added, 2.5 cm3 buffer solution and 2 drops of (EBT) indicator.

5.The EDTA solution was titrated until the dark colour turns blue.

6. The titration was repeated three times and the average concentration of the EDTA solution was find.
b. The determination of Zn solution concentration

1. 12.5 cm3 of Zn2+ solution was pipette into a 250 cm3 Erlenmeyer flask

2. 5cm3 of buffer solution was added and 2 drop of indicator.

3. Titrated with standard EDTA until the dark red colour turns blue. Slowly titrated and carefully towards
the end point.

4. The titration was repeated two or three times.

5. The concentration of Zn2+ in g dm-3 was calculated.


6.0 RESULTS AND CALCULATION

Part B. Standardization of EDTA solution


Reading taken 1 2 3

Initial Reading(cm3) 0.00 0.30 0.00


Final Reading (cm3) 13.00 13.40 13.40

Volume EDTA used (cm3) 13.00 13.10 13.40


Standard deviation 0.120 0.049 0.162

Average volume of EDTA used :

13.00+13.10+13.40
Avg =
3

= 13.17

∑(𝑣1 −𝑣𝑎𝑣𝑔 )2
Standard deviation = √
𝑛−1

∑(13−13.17)2
1. SD = √ 3−1

= 0.12

∑(13.10−13.17)2
2. SD = √ 3−1

=0.049

∑(13.40−13.17)2
3. SD =√ 3−1

= 0.162
C. Determination of Zn solution concentration

Reading taken 1 2 3
Initial Reading KMnO₄ (cm3) 0.00 0.00 0.00
Final Reading KMnO₄ (cm3) 44.1 42.6 43.3
Volume of EDTA used (cm3) 44.1 42.6 43.3
Standard deviation 0.544 0.516 0.021

Average volume of EDTA used :

44.1+42.6+43.3
Avg =
3

= 43.33

∑(𝑣1 −𝑣𝑎𝑣𝑔 )2
Standard deviation = √ 𝑛−1

∑(44.1−43.33)2
1. SD = √ 3−1

= 0.544

∑(42.6−43.33)2
2. SD = √ 3−1

=0.516

∑(43.3−43.33)2
3. SD =√ 3−1

= 0.021
6.1 Calculation

PART A: Preparation of EDTA 0.1 M

1. Formula of EDTA: C10H16N2O8. 2h20

The structure of EDTA

2. The molar mass of EDTA

RMM = (12.0107 x10) + (1.00794 x 18) + (14.0067 x 2) + (15.9994 x 10)+( 23 x 2)

= 372 g/mol

3. Number mole of EDTA

mass (g) 9.5 𝑔


g =
molar mass( ) 372 𝑔/𝑚𝑜𝑙
mol

= 0.0255 mol

4. Molarity of EDTA

Number of mole(mol) 0.0255 𝑚𝑜𝑙


=
Volume(dm3) 0.250 𝑑𝑚3

= 0.102 M
Part B : Standardization of EDTA solution

1. Concentration of Ca2+ solution

Let a =EDTA, b=Ca2+

MaVa =MbVb

(0.102 M)(0.01317)=Mb (0.0625)

Mb = 0.0214 M

2. Amount of Ca2+

𝑀/𝑣𝑜𝑙𝑢𝑚𝑒
No.of mole =
1000
0.0214/50
= 1000

=1.0746 x10-3 mol


3. Concentration of EDTA solution
𝑛
MEDTA = 𝑣
0.0255
=
0.01317

=1.94 M

Part C : Zn solution concentration

1. Equation of reaction

Zn2+ + 𝐸𝐷𝑇𝐴4− → (𝑍𝑛 (𝐸𝐷𝑇𝐴))2−

1 mol of Zn2+ reacted with 1 mol of EDTA


2. Concentration of Zn2+

Let a=EDTA , B=Zn2+

MaVa =MbVb

( 0.112 ) (43.33) =Mb (12.5 cm3)

Mb = 0.388 M

3. No of mole Zn2+

𝑚𝑜𝑙 43.33
= 0.388 ( ) dm3
𝑑𝑚3 1000

= 0.0168 mol
7.0 DISCUSSION
Complexometric titration is a form of volumetric analysis in which the formation of a colored
complex is used to indicate the end point of a titration. Complexometric titrations with EDTA have
traditionally been performed in undergraduate analytical chemistry courses to determine the calcium or
magnesium content of water. These titrations are performed at a basic pH, where the formation constants
of Ca-EDTA and Mg-EDTA complexes are high. These types of problems are well-treated in the analytical
chemistry textbooks. In contrast, treatment of metal ions whose EDTA complexes occur significantly at
low pH (e.g., Zn2+, Fe3+, Cu2+, Ni2+, Pb2+, Al3+) is sparse. An incorrect conclusion can be reached by
the student that practical EDTA titrations are only performed at high pH. In addition, widening the window
of possible metal ions for complexometric titration affords the possibility of analyzing real world products,
such as the cold lozenges discussed in the article

In this experiment, we first have to find the unknown concentration of the calcium solution from
the standardization by EDTA. We used at first 9.50g of EDTA salt to give 0.0255M of EDTA solution
before diluted. After Part B is conducted, the concentration of calcium solution obtained is 0.0214 M and
its amount calculated is 0.0010746 mol. After the addition of magnesium complex solution, buffer
solution and 1-2 drops of (EBT)indicator into the standard solution, the colour changed to dark purple. A
little of magnesium complex solution added to the calcium solution before the titration to initiate the rate
of reaction between EDTA and the metal solution.

After all, the average EDTA solution used to turn the dark colour to blue (end-point) in Part B is
13.17 cm3 with 0.11 deviation between its three consecutive repetition of the titration. The concentration
of EDTA that determined in Part B is 1.94M. Meanwhile, in Part C, we want to determine the
concentration of zinc solution using the concentration of EDTA obtained previously. In this part, the
average volume of EDTA used is 43.33 cm3 with its deviation 0.7506 less than 3 parts per thousand
which meant it is high accuracy titration. The concentration of zinc solution is 0.388 M in mol/dm3.

The two known systematic errors that came were measuring the solution as the eyes is not
perpendicular to the scale reading or from measurement error of the titrant as too much may have been
added.Possible sources for random error may have been from not measuring correctly.
The complexation of EDTA can also be applied in the field of medicine.It is used specifically to
detoxify patients poisoned with lead, mercury or arsenic which are converted by EDTA into a form that can
be excreted by the body without interacting first with the body.It the field of analytical chemistry, it is used
to bond with metal cations to prevent the interference of these to the desired reaction.

8.0 PRECAUTION STEP

1. Rinse all the apparatus that want to be used with the distilled water followed by respective chemicals
that to be filled in.

2. Shaking of the titration flask should be continous during adding the solution from the burette.

3. Always read lower meniscus in case of colourless solution and upper meniscus in case of coloured
solutions.

4. Keep your eye in level with the liquid surface while taking the burette reading or while reading the
pipette or measuring flask

5. Do not waste your time in bringing the burette reading to zero before each titration.

6. Usually an air bubble is present in the nozzle of the burette,it must be removed before taking the initial
reading.
9.0 CONCLUSION
The hypothesis for this experiment was to determine if complexometric titration technique can
identify the total “hardness” of water through mathematical means.Complexometric titration is the
titration that involved it titrant, a ligand, to reacts with the analyte, a metal ion, to form a complex, more
specifically a chelate in this case. A chelate is a ligand that has two or more sites that bind to the central
ion. EDTA react with almost all metal cation. For this experiment, it shows that EDTA react with calcium
and zinc metal. Futher applications of EDTA and other complexometric titration can be very useful in
industrial and other health aspects. Experimenters are now able to learn the basics and technique in this
kind of titration.

10.0 REFERENCE

1. D. A. Skoog, D. M. West, F. J. Holler, and S. R. Crouch, Analytical Chemistry: An Introduction, 7th

ed. Chapter 15, pp. 345-381.

2. Vogel's Textbook of Qualitative Inorganic Analysis by Vogel, A.I., 3rd, Ed., Longman (1961) 444,

445.

3. Gary D.Christian: Analytical Chemistry Sixth Edition, by John Wiley and Sons Inc.

4. https://www.quora.com/What-is-the-precaution-during-titration

5.https://www.researchgate.net/publication/231264560_The_Softening_of_Hard_Water_and_Complex

ometric_Titrations_An_Undergraduate_Experiment
11.0 Additional Question :

1. Why must we use buffer solution in titration involving EDTA.


The buffer adjusts the pH to ensure that the reaction goes to completion. EDTA, often written as H4Y , is
a common ligand in complexometric titrations. It has four carboxyl groups and two amine groups that can
act as electron pair donors (Lewis bases). EDTA is often used as the disodium salt, Na2H2Y . Carrying
out the reaction in a basic buffer solution removes the H+ as it is formed. Carrying out the reaction in a
basic buffer solution removes theH+ as it is formed.This moves the position of equilibrium to the right
and favours formation of the complex (Le Châtelier's Principle).Also, for EDTA, pKa4 = 10.26.Thus, if
the solution is buffered to about pH 10.3, most of the EDTA will exist as Y4-ions.The metal ions will not
have to remove the hydrogen ions from H2Y2-. They can react directly according to the equation

M2++Y4-→MY2-

Above pH 10.3, most metal ions react quantitatively with EDTA. Buffer solution must be used in
titrations involving EDTA because we need to constant the pH value of the metal solution around pH10
so that the complex formation will be quantitative.

2.Give examples of other indicators which may be used in EDTA titration.

 Calcein with EDTA for calcium


 Eriochrome Black T for calcium, magnesium and aluminium
 Fast Sulphon Black with EDTA for copper
 EGTA
 CDTA