Determination of Hardness in Water Lab Report

INTRODUCTION
Our Earth’s surface is approximately covered by 75% of water. The ocean holds about
97% of the Earth’s water surface, 2% is found locked in the polar ice caps and less
than one percent is available as fresh water for cooking, domestic uses, drinking and
others. Fresh water which originates from the rivers, streams, lakes and groundwater
contain relatively high concentrations of ions such as calcium and magnesium ions
but with a very little content of salt. Generally, high mineral content of these ions
especially calcium and magnesium ions in water is called hard water. Hardness in
water is caused polyvalent metallic cations even though the calcium and magnesium
ions (divalent cations) usually the predominant that cause hardness in water. Hardness
of water is the measure of its capacity to precipate soap. Hardness of water are
classified into two categories which is temporary hardness and permanent hardness.
Temporary hardness contains bicarbonates of calcium and magnesium which can be
removed easily by boiling whereas permanent hardness contains chlorides and
sulphates of calcium and magnesium which cannot be removed by boiling. For
instance, when the hard water is heated, calcium ions (Ca 2+) react with bicarbonates
(HCO3-) to form insoluble calcium carbonate ( CaCO3 ) which is known as scale.
Ca2+ (aq) +2 HCO3- (aq) → CaCO3 (s) + H2O + CO2
These cations ( calcium and magnesium ions) forms insoluble salt ( precipitate) with
an ordinary soap thus decreasing its cleaning effectiveness. Water hardness can be
represented in terms of mg calcium carbonate per litre of water (mg/L). The standard
way to express water hardness is in ppm CaCO3. Certain indicators are used in order to
determine hardness in water. However, the best way to determine
hardness in water is to perform a complexometric tiltration by using a standard
ethylenediamminetetraacecetic acid (EDTA) solution. This method is also used to
determine the metal ions present in the solution. In complexometric tiltratrion, EDTA
forms six bonds with metal ions to form one complex ion (complex tiltrations). A
metal indicator is used to determine the equivalence point.
In this experiment, hardness of unknown water samples are determine by performing
tiltrations with EDTA solutions .
OBJECTIVE
To determine the total hardness, calcium hardness and magnesium hardness of
unknown water samples .
APPARATUS
 Measuring cylinder (50ml)
 Conical flask (100ml) x 4 units
 Burette
 Retort stand and clamp
 Wash bottle with deionised water
 Dropper
 Spatula
MATERIALS AND CHEMICALS
 Eriochrome Black T
 Ammonium buffer solution, NH3OH and NH4Cl ( pH10 )
 0.01M EDTA
 4N Sodium hydroxide solution, NaOH
 Murexide (ammonium purpurite)
METHODS
Part A : Analysing Total Hardness of Water Sample A
1) 25ml of raw water sample A was measured using the 50ml measuring cylinder and
was transferred into a clean 100ml beaker.
2) The 50ml burette was cleaned and rinsed with distilled water to remove impurities
3) The burette was mounted to the retort stand and clamp.
4) The burette was filled with prepared 0.01M EDTA solutions to exact mark
measurement using filter funnel.
5) About 1 to 2 ml of prepared ammonia buffer solution, NH3OH and NH4Cl was
added into the 100ml beaker containing the water sample in order to make the
solution to pH10.
6) About 0.2g of Erichrome Black T indicator was added into the beaker.
7) The solution in the beaker was stirred well and the colour of the solution was
observed. A wine red solution was formed.
8) The solution was transferred into 100ml conical flask before starting to tiltrate
9) The initial volume of EDTA solution was read by recording the position of mark
that line up with the meniscus of the liqiud column.
10) 0.01M EDTA solution from the burette was slowly added into the conical flask
till the color of the solution changes from red wine to blue which indicate the reaction
has reached the end point.
11) The final volume of EDTA solution in the burette was recorded and total hardness
was calculated.
Part B : Analysing Calcium Hardness of Water Sample B

1) 25ml of raw water sample B was measured using the 50ml measuring cylinder and
was transferred into a clean 100ml beaker.
2) About 1-2 ml of sodium hydroxide, NaOH buffer and 0.1 murexide indicator was
added into 25ml of raw water sample.
3) The solution in the beaker was stirred well and the colour of the solution was
observed. A purple solution was formed.
4) The solution was transferred into 100ml conical flask before starting to tiltrate
5) The initial volume of EDTA solution in the burette was read by recording the
position of mark that line up with the meniscus of the liqiud column.
6) 0.01M EDTA solution from the burette was slowly added into the conical flask till
the color of the solution changes from purple to violet which indicate the reaction has
reached the end point.
7) The final volume of EDTA solution in the burette was recorded and calcium
hardness was calculated.
RESULTS
Part A : Tiltration of Water Sample A with EDTA solution
First reading Second reading Third reading
Initial burette reading (ml) 0.00 2.00 3.90
Final burette reading (ml) 2.00 3.90 5.70
Volume of EDTA used (ml) 2.00 1.90 1.80
Indicator used : Eriochrome Black T

Observation : The solution changes from wine red to blue
Wine red Blue
Average volume of EDTA used = 2.00 ml + 1.90 ml+ 1.80 ml

3
= 1.90 ml
Calculations of Total Hardness :

At the end point = milimoles of EDTA = milimoles of CaCO3
= M (EDTA) × V (EDTA)
= 0.01 × 1.90
= 0.019
Weight of CaCO3 = M (EDTA) × V (EDTA) × (MW of CaCO3)
= 0.01 × 1.90 × 100.0869
= 1.90165 mg
25ml
= 0.07607 × 1000
= 76.070 mg/L
= 76.070 ppm
Part B: Tiltration of Water Sample B with EDTA solution

First reading Second reading Third reading
Initial burette reading (ml) 0.00 1.30 2.50
Final burette reading (ml) 1.30 2.50 4.20
Volume of EDTA used (ml) 1.30 1.20 1.70
Indicator used : Murexide ( ammonium purpurite )

Observations : The solution changes from purple to violet
Purple Violet
Average volume of EDTA used = 1.30 ml + 1.20 ml+ 1.70 ml

3
= 1.40 ml
Calculations of Calcium Hardness :

At the end point = milimoles of EDTA = milimoles of CaCO3
= M (EDTA) × V (EDTA)
= 0.01 × 1.40
= 0.014
Weight of CaCO3 = M (EDTA) × V (EDTA) × (MW of CaCO3)
= 0.01 × 1.40 × 100.0869
= 1.40122 mg
25ml
= 0.05605 × 1000
= 56.050 mg/L
= 56.050 ppm
Magnesium Hardness as mg/L CaCO3 = Total Hardness - Calcium Hardness
= 76.070 - 56.050
= 20.020 mg/L
= 20.020 ppm
DISCUSSIONS
For Part A, the addition of ammonia buffer solution to raw water sample A does not
change the colour of solution and remains colorless. However, the addition of a small
quantity of Erichrome Black T indicator into the solution turns it to wine red. Upon
tiltrating the wine red solution with EDTA, the solution turns to blue. EDTA is a
chelating agents which forms stable complex ions with Ca 2+ and Mg2+ which is found
in the water sample. Eriochrome Black T indicator is used to show when all the ions
responsible for water hardness are consumed. Once Eriochrome Black T indicator is
added to water sample A with pH 10, it combines with Ca 2+ and Mg2+ ions forming a
weak complex ion which appears to be wine red in color. Upon tiltration, EDTA
disrupts the wine red complex since it can form a more stable complex ion with the
Ca2+ and Mg2+ ions thus changing the solution from wine red to blue indicating the
end of tiltration.
For Part B, the addition of sodium hydroxide buffer to raw water sample B does not
change the colour of solution and remain colorless. However, the addition of a small
quantity of murexide into the solution turns it to purple. Upon tiltrating the purple
solution with EDTA, the solutions turns to violet. Murexide is a metallochromic
indicator which undergoes color changes in the presence of calcium ions. Calcium
hardness are determined by raising the pH value of water sample B in which
magnesium ions are precipitated and EDTA forms a stable complex ion with Ca 2+.
Thus, it results in changes in color of the solution from purple to violet when
murexide is used as indicator.
Table below shows how water is classified based on the hardness scale.
Total Hardness ( mg/L as CaCO3 )

Soft 0-30
Moderately soft 30-60
Moderately hard 60-120
Hard 120-180
Very Hard > 180
The total hardness obtained for water sample A from Part A is 76.070 mg/L ( 76.070
ppm). The calcium hardness obtained for water sample B from Part B is 56.050 mg/L
(56.050 ppm). The difference between total hardness and calcium hardness is the
magnesium hardness which is 20.020 mg/L (20.020 ppm). Based on the total hardness
obtained, the water sample is considered as moderately hard as it exceeds 60.000
mg/L.
CONCLUSION
The water sample obtained is considered as moderately hard as the total hardness
obtained exceeds 60.000mg/L. The total hardness obtained is 76.070 mg/L , calcium
hardness is 56.050 mg/L and magnesium hardness is 20.020 mg/L. Complexometric
tiltration is a method used to determine the hardness of water of an unknown sample.
There are several precautionary steps to be follow when conducting the experiment.
 The eyes must be placed exactly at the level of meniscus when taking the reading
of burette.
 Always rinse the burette with the solution, which is to be taken in it.
 Before tiltrating the solution, make sure to remove the air gap from the burette if
any and make sure the nozzle of burette is also filled.
 Never use the pipette and burette with a broken nozzle.
 Always keep the lower end of the pipette dipped in the liqiud while sucking the
liqiud.
REFERENCES
https://www.studocu.com/en-us/document/mesa-community-college/general-
chemistry-ii/water-hardness-lab-report/7310953

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INTRODUCTION

Part B : Analysing Calcium Hardness of Water Sample B

Indicator used : Eriochrome Black T

Average volume of EDTA used = 2.00 ml + 1.90 ml+ 1.80 ml

Calculations of Total Hardness :

Part B: Tiltration of Water Sample B with EDTA solution

Indicator used : Murexide ( ammonium purpurite )

Average volume of EDTA used = 1.30 ml + 1.20 ml+ 1.70 ml

Calculations of Calcium Hardness :

Total Hardness ( mg/L as CaCO3 )

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