Experiment 5 Sku3033

EXPERIMENT 5 - DETERMINATION OF CHLORIDE ION IN WATER
5.1 OBJECTIVES
Upon completion of this experiment, students should be able to:
1. determine the chloride ion in water sample
5.2 INTRODUCTION
Chloride ion is essential to the electrolytic balance in our bodies. Since there is a
continous intake and excretion of chlorine from all animals, it is one of the most
abundant anions found in wastewater and is a good marker ion for pollution sources.
Chloride gives water a salty taste, detectable at a level of 250 ppm if the cation
present is sodium. With calcium and magnesium as counter ions, this salty taste is
not detectable until the chloride concentration reaches up to 1000 ppm. High chloride
levels can pose a threat to crops and freshwater aquatic plants, which do not have
mechanism to excrete excess of salt. High levels of chloride in a water system
increase the rate of corrosion of metallic pipes.
MOHR’S method
The chloride present in the water sample in titrated with silver nitrate solution.
Cl- + Ag+  AgCl (Kw = 3 x 10-10)
Potassium chromate is used as an indicator. At the end point, the concentration of

chloride ion in solution approaches zero and the silver ion concentration increases to
a level at which solubility product of silver chromate is exceeded. Then, silver
chromate is precipitated as a reddish-brown product.
2Ag+ + CrO42- ↔ Ag2CrO4 (Kep = 5 x 10-12)
The appearance of reddish-brown colour signals the end point. A small excess of Ag+
is required to produce a visible quantity of Ag 2CrO4; therefore, an indicator correction
has to be made in the titre value by performing blank titration.
The pH of the water sample should be in the 7-8 range; when it is less, CrO 42- is
converted to Cr2O72-; when it is more , Ag+ is precipitated as AgOH.
For all the titrations, a definite volume of the indicator should be accurately pipetted
into the analyte.
5.3 MATERIALS
Distilled water
Standard sodium chloride solution (0.005 M)
Silver nitrate solution (0.005 M)
Potassium chromate indicator
5.4 APPARATUS
Erlenmeyer flask
Volumetric flask
Burette
Retort stand
White tiles
Filter funnel
Pipette
Pipette Bulb
Dropper
5.5 METHODS
1. 100 mL water sample was pipetted into an Erlenmeyer flask. 1 mL K2CrO4

indicator pipetted into it.
2. The solution was titrated with the standardized silver nitrate solution. The end
point is the appearance of reddish-brown colour.
3. A duplicate titration was duplicated in an identical manner.
4. A blank titration was carry out using 100 mL deionized, chloride-free water and
1mL indicator. This titre value subtracted from that obtained for the water sample
for indicator correction.
5.6 RESULTS
Sample A : Tap water
Trial 1 2
Initial (mL) 0.00 8.60

Final (mL) 8.40 15.60
Volume (mL) 8.40 7.00
Volume Average
(mL) 7.40
Observation - colour Yellow → Reddish-brown

change
Sample B : Cuckoo water
Trial 1 2
Initial (mL) 15.60 23.10

Final (mL) 23.10 30.50
Volume (mL) 7.50 7.40
Volume Average
(mL) 7.45

change
Sample C : Distilled water
Trial 1 2
Initial (mL) 30.60 34.50

Final (mL) 34.50 36.80
Volume (mL) 3.90 2.30
Volume Average
(mL) 3.10

change
5.7 CALCULATION
Calculation of chloride concentration in water:
From 1000 mL of 1.0 M AgNO3 it has 35.45 g of Cl- ions
a) Mass of chloride ions in mg = A mg
b) The amount of chloride (in mg L-1 or ppm) in water sample
A V 2  M
= V1
Where
Sample A : Tap water
Sample B : Cuckoo water
Sample C : Distilled water

5.8 DISCUSSION
From this experiment, sample A (Tap water) containing the highest amount of
chloride ion more than others, which is 13.65 ppm of Cl- while sample B (Cuckoo)
containing 13.21 ppm of Cl- and sample C (distilled water) containing 5.49 ppm of Cl-.
In this experiment, the titration of water sample was conducted in the pH range of 7
to 8. This is because at pH lower than 7, the chromate ion will be converted to
dichromate ion.
CrO42-(aq) → Cr2O7- (aq)
Eventually, this dichromate ion cannot form a brick red silver chromate precipitate
with silver ion and hence end point of the titration cannot be detected. At pH higher
than 8, the silver ion will tend to react with the excess hydroxide ion to form browish
silver hydroxide. Formation of silver hydroxide will cover the colour of silver chromate
precipitate and hence the end point also cannot be seen.
Ag+(aq) + OH-(aq) → AgOH (s)
MOHR method can only roughly show the concentration of chloride ion in water
sample. This is because excess silver nitrate is needed to produce sufficient silver
chromate precipitate to be observed in the solution with heavy white precipitate of
silver chloride. Besides, the intense yellow colour of chromate solution causes the
brick red silver chromate that formed is hardly to be observed.
There are some precaution steps need to take for this experiment to avoid errors
occur. First of all, all solution mixture that involved silver nitrate solution must be
discarded into waste bottle because silver is heavy metal. Next, the burette must be
rinsed with silver nitrate solution before titration starts. Then, wear gloves when
handling silver nitrate solution since it will cause skin staining and chemical burn.
Lastly, chromate solution needs to be used with care as chromate is a known
carcinogen.
5.9 CONCLUSION
As a conclusion, tap water containing higher concentration of chloride ion than

Cuckoo water and distilled water. Chloride is also a useful and reliable chemical
indicator of river or groundwater fecal contamination, as chloride is a non-reactive
solute and ubiquitous to sewage & potable water. Many water regulating companies
around the world utilize chloride to check the contamination levels of the rivers and
potable water sources.
5.10 REFERENCES
1. http://1chemistry.blogspot.com/2013/07/determination-of-chloride-ion-in.html
2. Laboratory manual Environmental Chemistry.

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EXPERIMENT 5 - DETERMINATION OF CHLORIDE ION IN WATER

Upon completion of this experiment, students should be able to:

1. determine the chloride ion in water sample

Cl- + Ag+  AgCl (Kw = 3 x 10-10)

Potassium chromate is used as an indicator. At the end point, the concentration of

2Ag+ + CrO42- ↔ Ag2CrO4 (Kep = 5 x 10-12)

1. 100 mL water sample was pipetted into an Erlenmeyer flask. 1 mL K2CrO4

3. A duplicate titration was duplicated in an identical manner.

Sample A : Tap water

Initial (mL) 0.00 8.60

Observation - colour Yellow → Reddish-brown

Sample B : Cuckoo water

Initial (mL) 15.60 23.10

Observation - colour Yellow → Reddish-brown

Sample C : Distilled water

Initial (mL) 30.60 34.50

Observation - colour Yellow → Reddish-brown

Calculation of chloride concentration in water:

From 1000 mL of 1.0 M AgNO3 it has 35.45 g of Cl- ions

a) Mass of chloride ions in mg = A mg

b) The amount of chloride (in mg L-1 or ppm) in water sample

Sample A : Tap water

Sample B : Cuckoo water

Sample C : Distilled water

CrO42-(aq) → Cr2O7- (aq)

Ag+(aq) + OH-(aq) → AgOH (s)

As a conclusion, tap water containing higher concentration of chloride ion than

2. Laboratory manual Environmental Chemistry.

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