MIDLANDS STATE UNIVERSITY

MANICALANDS COLLEGE OF APPLIED SCIENCES

DEPARTMENT OF CHEMICAL AND PROCESSING SYSTEMS
ENGINEERING
BSc(Hons) Chemical and Processing Engineering
HCHE 222 ANALYTICAL CHEMISTRY
Name:

Panashe Muduzu

Reg #:

R14966Z

Level:

2.2

Title:

EDTA Titration

Practical Number:

Partner(s):

Kudakwashe Dengure
Tafadzwa Mukwazhi
Tapiwa Tokwe

Lecturer:
Date:

Dr I Nyambiya
22 June 2016

Aim:
To determine Calcium hardness in borehole water and concentration of
Nickel in a sample solution using EDTA titrations.
Objectives:
1. A primary-standard zinc ion solution will be prepared from primarystandard zinc metal.
2. A supplied EDTA solution will be standardized
using the primary-standard zinc ion solution.
3. A secondary standard EDTA solution will be employed to determine the
amount calcium ion in borehole water
4. A secondary standard EDTA solution will be employed to determine
concentration of nickel in a sample solution

ABSTRACT
In this experiment harness of borehole water and concentration of nickel
in an unknown sample will be determined. The calcium content will be
determined by performing titration with standardised EDTA. Eriochrome
black T will be used as an indicator. The molarity of nickel is also to
determine by titration with standardised EDTA. Murexide is to be used as
the indicator. EDTA is to be standardised using ZnO solution. Calcium
water hardness was found to be 251.60 ppm and concentration of nickel
was 0.001423 M.
LITERATURE REVIEW
Ethylenedinitrilotetraacetic acid (EDTA: 1,2 diaminoethanetetra-acetic
acid), 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.
-

HOOCH2C
CH2COOH
CH2-COO

OOC-CH2

N-CH2-CH2-N

HOOCH2C
CH2-COO-

N-CH2-CH2-N

CH2COOH

OOC-CH2

The ion is a hexadentate ligand and one of its most interesting features is
that it forms 1:1 complexes with metal ions regardless of their charge. .
When a solution containing a suitable divalent metal ion is titrated with
EDTA , the reaction that occurs can be formulated:
M2+

H2Y2

MY2-

2H+

The above process is called chelation and the chelation reaction between
EDTA and many metal ions has a very large equilibrium constant.
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.

The end-points of titrations with EDTA are usually detected by

metallochromic indicators. These are organic colourship matters that
undergo a colour change when they form metal complexes. Two of the
most common metallochromic indicators are murexide and eriochrome
black T (Erio T for short).
Murexide , which is blue in alkaline solution , forms a pink complex with
calcium ions . When a solution containing calcium and murexide is titrated
with EDTA, EDTA will react with all the metal ions thus removing them
from murexide and all the original blue color of the indicator is restored.
The structure of murexide is shown below:

Erio T is a complexometric indicator that is used in complexometric

titrations, e.g. in the water hardness determination process. It is an azo
dye. Erio T indicator is blue between pH 6.3 and 11.3 and it turns wine
red when it forms a complex with calcium and other metal ions. When a
solution containing erio T and calcium is titrated with EDTA the blue colour
of the indicator restored after all the metal ions have been complexed.
The structure of erio T is given below:

EDTA titrations can be used to determine water hardness and find

concentration of metal ions in a solution among others. In this experiment
complexometric titration will be used to determine borehole water
hardness in ppm and molarity of nickel ions in a sample solution.
PRECAUTIONS AND SAFETY

NH3 causes irritation when inhaled thus NH3 buffer should be added
to the sample in a fume exhaust hood and the solution should be
brought back to the working bench after complete dilution.
EDTA should be kept in a resistant glass or plastic container to avoid
leaching of calcium ions.

Safety goggles, safety shoes, lab coat and latex gloves should be
worn all the time
Use a funnel to add titrant to the burette and place the top of
burette below eye level when filling it.
Turbid buffer solution must be discarded

The following errors might be encountered in the experiment:

Parallax error and it can be minimised by following the correct

procedure when takin reading from instruments
Systematic error and can be minimised by comparing your results
with others obtained independently, using different equipment or
calibrating instruments before use
Operational error, this is minimised by giving your undivided
attention to practical details.
Using wrong amount of indicator - in the case of single colour
indicators amount added can shift end point. It can be avoided by
following the practical procedure.
Using contaminated solutions - for example when two different
solutions are transferred using the same pipette and pipette is not
rinsed with distilled water in between.

APPARATUS
Droppers, 250ml volumetric flasks, 10ml and 50ml pipette, 50ml burette,
250ml conical flasks, spatula and beakers
Reagents
Chemical name

Chemical
formula

Manufacturer

Mass/
concentration

Concentrated
ammonia

NH3

SCIENTIFIC MASTERS

25%

Sodium sulphide

Na2S

ALPHA CHEMIKA

1%

Ammonium
chloride

NH4Cl

ASSOCIATED CHEMICAL
ENTERPRISES

1M

Murexide

NH4C8H4N5O6

RIEDEL DE HAN

Hydrochloric acid

HCl

ASSOCIATED CHEMICAL
ENTERPRISES

0.5M

EDTA

C10H16N2O8

SKYCHEM

0.05062 M

Erio T

C20H12N3O7SNa GLASS WORLD

Zinc oxide

ZnO

SKY CHEM

0.25g

Instrumentation
Name

Model

Manufacturer

Use in the
practical

Weighing balance

JJ224BC

G&G

To measure mass
of ZnO

PROCEDURE
Standardization of EDTA solution
0.25 g of ZnO was weighed and transferred into a conical flask. 0.5 M HCl
was added dropwise until all ZnO dissolved. The solution was then cooled
and transferred into a 250ml volumetric flask and filled to the mark with
distilled water. 10ml portions were pipetted each into 250ml conical flasks
concentrated ammonia was added in excess to dissolve the precipitate
formed. The solution was then titrated with EDTA using Erio T indicator.
Determination of Ca Hardness in water
100ml of bore-hole water were pipetted into a 250ml conical flask, 2ml of
the ammonia buffer pH 10 and add 2 drops of freshly prepared 1% sodium
sulphide solution were added. After 1 minute 4 drops of Erio T indicator
were added and titrated with the standardized EDTA solution until the last
traces of red had disappeared from the solution.
Determination of Nickel
100ml of the neutral sample solution were pipetted into a 250ml conical
flask and murexide indicator was added. Then 10 ml of 1M NH4Cl were
added. Dilute ammonia was added dropwise until the colour changed
from orange-yellow to yellow. Titration was done until the end-point was
near with addition of a few drops of ammonia when the colour reverted to
orange and titration continued. Just before the end-point the solution was
made strongly ammonical by adding 10ml of concentrated ammonia and
titrated to a brilliant colour change from yellow to bluish-violet.
DATA TREATMENT
1. Zinc ion react with EDTA as follows:
2
4 Zn(EDTA )
2++ EDTA
Zn
the reaction between EDTAall meta ionsis 1 mol 1mol

2+
Zn

n
n ( EDTA ) =0.00318
From experiment 1:
average volume of EDTA solutionused =

2.1+2.1+2.1+2.2
=2.10 ml
4

molarity of EDTA=(n ( EDTA )DILUTION RATIO)/volome of EDTA

0.0031810
1000
250
=0.06057
2.1

= 0.06057 M
2. Ca Hardness of borehole water
2
4 Ca( EDTA)
2++ EDTA
Ca
reactionratio is 1: 1
From experiment 2:
average volume of EDTA used =

4.1+4.2
=4.15 ml
2
2+

Ca

n ( EDTA )=n

0.060574.15
=2.51104
1000
= 2.51*10-4

M r of CaC 0 3=100.0869 g /mol

2+
Ca

) = 2.51 * 10-4 *100.0869

CaCO3
2+ =n

mass of Ca
= 25.160 mg
Volume of water used = 100 ml

2+
Ca /mg

mass
total hardness=
=
25.1601000
=251.60 ppm
100
3. Concentration of nickel in sample solution
2
4 ( EDTA)
2+ + EDTA

reactionratio 1 :1
From experiment 3:
average volume of EDTA used =

2.2+2.5
=2.35 ml
2

2+

n ( EDTA )=n

2.35
( 1000
)=1.42310

0.06057

mols
Volume of sample solution used (v) = 100 ml
2+

n
concentrationof
DISCUSSION
Overally the aims and objectives of the experiment were achieved
successfully. The molarity was calculated from titration information and
was found as 0.06057 M. The Ca hardness of water was found to be
251.60 ppm. The hardness of water is structured by a numerical range.
Soft water has a ppm between 0 and 75. Moderately hard has a range of
75-150. Hard is between 150 and 300. Anything over 300 ppm is
considered very hard. The borehole water sample was in the hard range of
the scale. The concentration of Ni in the sample solution was 0.001423 M,
this implies that in every litre of the sample solution there are 0.001423

moles of nickel ions. The expected colour change from red to blue was
observed when ZnO solution was titrated with EDTA using Erio T indicator
during standardization of EDTA. The molarity was calculated and found to
be 0.05062 M which is fairly good when compared to theoretical values.
Furthermore another colour change from red to blue was observed in the
titration of calcium ions solution with EDTA using Erio T indicator.
Moreover when murexide indicator was used in the titration of a sample
solution containing Ni ions with EDTA a brilliant colour change from yellow
to bluish-violet was observed thus proving to be in consistency with
theoretical expectations of the titrations.
It is important to determine the hardness of water especially in
residences because hard water can cause problems in home and even in
industries. When reacted with soap, precipitates of Ca 2+ andMg2+ salts
form. This causes the soap to lose some of its effectiveness as a cleaning
agent and the precipitates form scum that stick to cloth, sinks and
bathtubs. Ca2+ and Mg2+ carbonates can also precipitate and form boiler
scales in water pipes, commercial boilers and other vessels. In this case,
the water sample is moderately hard, making it unadvisable to use in
household cleaning and boiling. 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. In the field of analytical chemistry, itis used to bond with metal
cations to prevent the interference of these to the desired reaction. Nickel
is a dietary requirement for many organisms, but may be toxic in larger
doses. Metallic nickel and some other nickel compounds are teratogenic
and carcinogenic to mammals thus it is of paramount importance to
determine amount of nickel in drinking water.
However the uncertainties that are associated with measuring
instruments could have affected the accuracy results obtained to a lesser
extent. For example the mass of ZnO measured was 0.2588 0.0001 g
and the volumes recorded from the burette had uncertainties

0.10

cm3.

Also there the accuracy of results might have by random errors such as
overshooting the endpoint of titration. This will result in an incorrect
volume reading.
CONCLUSION
The results from this experiment were reasonable. The molarity of EDTA
was determined by titration and was found to be 0.06057 M and borehole
water hardness was found to be 210.18 ppm which makes it fall in the
range of numbers indicating hard water. The concentration of nickel in the
sample solution was 0.001423 M which is a reasonable amount.
REFERENCES

i.
ii.
iii.
iv.

v.
vi.
vii.
viii.
ix.
x.

Skoog, et al., 2014, Fundamentals of Analytical Chemistry, 9 th

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