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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.
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
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
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
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
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.