Determination of Chlorides

DETERMINATION OF CHLORIDES
THEORETICAL BACKGROUND
Chloride (Cl-) occurs in all natural waters in widely varying

concentrations. It is one of the major inorganic anion in water and
wastewater. In potable water, the salty taste produced by chloride
concentrations is variant and depends on the chemical composition of
water. The chloride content normally increases with the mineral
contents of water. Chlorides in reasonable concentration are not
harmful to humans. Above 250 mg/L of Cl- in water may have a
detectable salty taste if the cation is sodium. On the other hand, the
typical salty taste may be absent in water containing as much as
1000mg/L when the predominant cations are calcium and magnesium.
The chloride concentration is higher in wastewater than in raw
water because sodium chloride is a common component of human
diet and passes unchanged through the digestive system into the
sewage. High Cl- concentrations in water are not known to have toxic
effects on man. The maximum allowable Cl- concentration of 250mg/L
in drinking water has been established for reasons of taste rather than
as a safeguard against physical hazards.
SOURCES OF CHLORIDES IN WATER
1. Cl- occurs in the form of minerals in earth curst, example:

(a). Rock salts: NaCl, (b). Carnallite: KCl.MgCl2.6H2O,
(c). Sylvite: KCl etc. These minerals when dissolve in water/ water
ground generate Cl-.
2. Industrial wastewater/effluent is another source of addition of Cl-
in water.
3. Chloride may be present in high concentrations along the
seacoast because of seepage of seawater.
ADVERSE EFFECTS OF CHLORIDES IN WATER
1. High chloride concentrations may cause corrosion of metallic

pipes and other metallic structures, resulting in water leakage.
2. High chloride concentration may also be harmful to plants. Plant
transpiration tends to increase the chloride (salinity) at the root
zone of irrigated plants, making it difficult for crops to take up
water due to osmotic pressure difference between the water
outside the plants and within the plant cells.
METHOD OF DETERMINATION: ARGENTOMETRIC METHOD
In this method, a water sample is titrated against a standardized

silver nitrate solution using potassium chromate as an indicator. It is
suitable for relatively clear waters. Silver nitrate first reacts selectively
with the chloride present in the sample to produce insoluble white silver
chloride. After all the chloride has been precipitated, the silver nitrate
reacts with potassium chromate to form pinkish-yellow silver chromate
precipitates, marking the end point of titration.
AgNO3 + K2CrO4 + Cl- AgCl + NO3- + K2CrO4

2AgNO3 + K2CrO4 Ag2CrO4 + KNO3
(Pinkish-yellow)
Samples must be titrated in the pH range 7-10 because Ag+ is

precipitated as AgOH at high pH levels. On the other hand CrO42- is
converted into Cr2O72- at low PH levels.
INTERFERENCE
Substances in amounts normally found in potable waters do not

interfere. Bromide, iodide and cyanide cause interferences to a great
extent. Sulfide, thiosulfate and sulfite ions interfere but can be removed
by treatment with hydrogen peroxide. Orthophosphate in excess of
25mg/L interferes by precipitating as silver phosphate. Iron in excess of
10mg/L interferes by masking the end point.
APPARATUS
Glassware, Burette, Volumetric Flask, Pipette, Magnetic Stirrer.
REAGENTS
a. Potassium Chromate Indicator Solution

Dissolve 50g of K2CrO4 in a little distilled water. Add AgNO3
solution until a definite red precipitate is formed. Let it stand for
12 hours, and dilute to 1L with distilled water.
b. Standard Silver Nitrate Titrant, 0.0141M (0.0141N)
Dissolve 2.395g of AgNO3 in distilled water and dilute to 1000mL.
Standardized against NaCl. Store in brown bottle.1mL = 0.5mg Cl-
c. Standard Sodium Chloride, 0.0141M (0.0141N)
Dissolve 0.824g of NaCl (dried at 140oC) in distilled water and
dilute to 1L. 1mL = 0.5mg Cl-
FOR REMOVAL OF INTERFERENCE
A. Aluminum Hydroxide Suspension

Dissolve 125g of aluminum potassium sulfate AlK(SO4 )2.12H2O or
aluminum ammonium sulfate AlNH4(SO4 )2.12H2O , in 1L distilled
water. Warm to 60oC and add 55mL of conc. NH4OH slowly with
stirring. Let it stand for 1hour. Then, transfer to a larger bottle, and
wash the precipitate by successive additions, with thorough
mixing and decanting with distilled water, until it becomes free of
chloride. When freshly prepared, the suspension occupies a
volume of approximately 1L.
B. Phenolphthalein Indicator Solution
C. Sodium Hydroxide, NaOH, 1N
D. Sulfuric Acid, H2SO4, 1N
E. Hydrogen peroxide, H2O2
SAMPLING AND STORAGE
Collect samples in clean plastic or glass bottles. Samples can be

stored in sealed containers.
PROCEDURE
I. Sample Preparation:
Use a 100mL sample or a suitable portion diluted to 100mL. If the
sample is highly colored, add 3mL of Al(OH)3 suspension, mix, let
it settle down, and filter. If sulfide, sulfite, or thiosulfate is present,
add 1mL of H2O2 and stir for 1minute.
II. Titration:
Directly titrate samples in the pH range 7 to 10. Adjust sample pH
in the range 7 -10 with H2SO4 or NaOH if not in this range. For
adjustments, preferably use a pH meter with non-chloride-type
reference electrode.
Steps
First standardize the silver nitrate solution (titrant) against a

primary standard NaCl solution (0.0141N) through titration. Calculate
the exact normality of AgNO3.
1. Select an appropriate sample volume and standard titrant
solution that corresponds to the expected chloride (Cl-)
concentration in the sample.
2. Use a graduated cylinder or pipette to measure the sample
volume (say 100mL).
3. Transfer the sample into a 250mL Erlenmeyer flask. Dilute to
100mL with deionized water if a small volume of the sample is
selected.
4. Add 1mL K2CrO4 indicator solution in the flask.
5. Fill a 50mL burette to the zero mark with the silver nitrate solution.
6. Titrate the sample while swirling the flask until the color changes
from yellow to pinkish-yellow.
7. Repeat the sample titration two more times and calculate the
mean volume of AgNO3 used.
8. Perform the above steps 3-6 using distilled water instead of the
sample to establish Reagent Blank value.
CALCULATION
Calculate conc. of Cl- ions in the sample as under.
mg Cl- /L = (A-B) x N x 35450

ml sample
Where A = ml titration for sample

B = ml titration for blank and
N = Normality of AgNO3

Determination of Chlorides

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DETERMINATION OF CHLORIDES

Chloride (Cl-) occurs in all natural waters in widely varying

SOURCES OF CHLORIDES IN WATER

1. Cl- occurs in the form of minerals in earth curst, example:

ADVERSE EFFECTS OF CHLORIDES IN WATER

1. High chloride concentrations may cause corrosion of metallic

METHOD OF DETERMINATION: ARGENTOMETRIC METHOD

In this method, a water sample is titrated against a standardized

AgNO3 + K2CrO4 + Cl- AgCl + NO3- + K2CrO4

Samples must be titrated in the pH range 7-10 because Ag+ is

Substances in amounts normally found in potable waters do not

Glassware, Burette, Volumetric Flask, Pipette, Magnetic Stirrer.

a. Potassium Chromate Indicator Solution

FOR REMOVAL OF INTERFERENCE

A. Aluminum Hydroxide Suspension

SAMPLING AND STORAGE

Collect samples in clean plastic or glass bottles. Samples can be

First standardize the silver nitrate solution (titrant) against a

Calculate conc. of Cl- ions in the sample as under.

mg Cl- /L = (A-B) x N x 35450

Where A = ml titration for sample

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