EXPT NO.

3 CHLORIDES AND SULPHATES

DETERMINATION OF CHLORIDES AND SULPHATES

AIM
To analyse the chemical characteristics of a given water sample viz. chlorides and sulphates for assessing its
suitability for drinking water purposes and building construction.
1. DETERMINATION OF CHLORIDES
Objective
To determine the chlorides of the given water sample.
Introduction
This method determines the chloride ion concentration of a solution by titration with silver nitrate. As the silver
nitrate solution is slowly added, a precipitate of silver chloride forms.
Ag+(aq) + Cl–(aq) → AgCl(s)
The end point of the titration occurs when all the chloride ions are precipitated. Then additional silver ions
react with the chromate ions of the indicator, potassium chromate, to form a red-brown precipitate of silver
chromate.
2 Ag+(aq) + CrO42–(aq) → Ag2CrO4(s)
This method can be used to determine the chloride ion concentration of water samples from many sources
such as seawater, stream water, river water and estuary water. Seawater is used as the example here.
The pH of the sample solutions should be between 6.5 and 10. At higher pH silver ions may be removed by
precipitation with hydroxide ions, and at low pH chromate ions may be removed by an acid-base reaction to
form hydrogen chromate ions or dichromate ions, affecting the accuracy of the end point used.
Environmental Significance
In potable water, the salty taste produced by chloride concentration is variable and depends on the chemical
composition of water. Some waters containing 250 mg/L Cl- may have a detectable salty taste if sodium cation
is present. On the other hand, the typical salty taste may be absent in waters containing as much as 1000 mg/L
when the predominant cations are calcium and magnesium. In addition, a high chloride contents may harm
metallic pipes and structures as well as growing plants. The measured chloride ions can be used to know
salinity of different water sources. For brackish water (or sea water or industrial brine solution), it is an
important parameter and indicates the extent of desalting of apparatus required. It also interferes with COD
determination and thus it requires a correction to be made on the basis of amount present or else a
complexing agent, such as HgSO4 can be added. Further, chloride ions are used as tracer ions in column
studies to model fate of different contaminants in soil and liquid media. For building construction, the
Chlorides (Cl) is as follows a) 1000 mg/l for RCC work and, b) 2000 mg/l for PCC work
Principle
The amount of chloride present in water can be easily determined by titrating the given water sample with
silver nitrate solution. The silver nitrate reacts with chloride ion according to1 mole of AgNO 3 reacts with 1
mole of chloride. The titrant concentration is generally 0.02 M. Silver chloride is precipitated quantitatively,
before red silver chromate is formed. The end of titration is indicated by formation of red silver chromate from
excess silver nitrate. The results are expressed in mg/L of chloride (Cl - with a molecular weight of 35.453
g/mol).
Materials Required
Apparatus Required
1. Burette with Burette stand
2. Pipette
3. Erlenmeyer flask
4. Wash Bottle
Chemicals Required
1. Silver nitrate
2. Phenolphthalein Indicator
3. Sodium chloride
4. Potassium chromate
Procedure
1. Take 20mL of sample (V) and dilute to 100mL.

DEPARTMENT OF CIVIL ENGINEERING, SNIT ADOOR

 EXPT NO. 3 CHLORIDES AND SULPHATES

2. If the sample is coloured add 3mL of aluminium hydroxide, shake well; allow to settle, filter, wash and
collect filtrate.
3. Sample is brought to pH 7-8 by adding acid or alkali as required.
4. Add 1mL of indicator (Potassium chromate).
5. Titrate the solution against standard silver nitrate solution until a reddish brown precipitate is
obtained. Note down the volume (V1).
6. Repeat the procedure for blank and note down the volume (V2).
Observations

Trial VOLUME OF THE SAMPLE BURETTE READING VOLUME OF

No. INITIAL FINAL AgNO3
1
2
B1
B2
Calculations
(𝑉1−𝑉2)𝑋𝑁𝑋35.45𝑋100
mg/L of Chloride = 𝑉
where
V1 = Volume in mL of standard Aluminium Nitrate used to titrate sample
V2 = Volume in mL of standard Aluminium Nitrate used to titrate blank
N = Normality of standard Sodium Hydroxide (N=0.0141)
V = Volume in mL of sample taken for test
Results
The chloride of the given sample =
Inference
The high concentrations of chloride ions mostly result in an unpleasant salty taste of water and it also aides the
corrosion of plumbing system. Very high chloride content of water may also produce laxative effect. An upper
limit of 250 mg/L has been set for the chloride ions. An increase in the normal chloride content of your water
may indicate possible pollution from human sewage, animal manure or industrial wastes. As all aware the sea
water is full of sodium chloride, the chloride levels will be much higher compared to the fresh water sources.
The given sample is having chloride content ___ than 250mg/L, so it is/not fit for drinking.

2. DETERMINATION OF
SULPHATES Objective
To determine the sulphates of the given water sample.
Introduction
Sulphates are found in appreciable quantity in all natural waters, particularly high in arid and semi-arid regions
where natural waters in general have high salt content. Sulphate salts are mostly soluble in water and impart
hardness. Water with high concentrations has a bitter test. Sulphate may cause intestinal disorders. These ions
can produce Hydrogen Sulphides as per following equation (1):
SO42-+organic matter  S2-+H2O+CO2 (1a) (in the presence of anaerobic bacteria)
S2-+ H+ HS- (1b)
HS-+ H+ H2S (1c)
The sulphate data is used in determining applicability of different water types for their public and industrial
applications. It indirectly indicates extent of problems that can arise due to reduction of sulphates to hydrogen
sulphides. Sulphate is the second most abundant anion in seawater. Its high concentration owes to the high to
moderate solubility of the salts that it forms with the major cations in seawater, namely, Na, Mg 2+, and Ca2+.
Environmental Significance
Sulphates are of considerable concern because they are indirectly responsible for two serious problems often
associated with the handling and treatment of wastewater. They are odour and sewer corrosion problem
result from the reduction of sulphates to hydrogen sulphide under anaerobic conditions.
The amount of sulphates in wastewater is a factor of concern in determining the magnitude of problems that
can arise from reduction of sulphates to hydrogen sulphide. For example, knowledge of the sulphates content
of the sludge or waste fed to digestion units provides a means of estimating the hydrogen sulphide content of

DEPARTMENT OF CIVIL ENGINEERING, SNIT ADOOR

 EXPT NO. 3 CHLORIDES AND SULPHATES

the gas produced. From this information, the design engineer can determine whether scrubbing facilities will be
needed to remove hydrogen sulphide and size of the units required.
Principle
The turbidimetric method of measuring sulphates is based upon the fact that barium sulphates tends to
precipitate in a colloidal form of uniform size and that this tendency is enhanced in the presence of an acidic
buffer (consists of magnesium chloride, potassium nitrate, sodium acetate, and acetic acid). These precipitates
need to be separated through filtration (using a filter) before sample is analysed for sulphate concentration.
This is a very rapid method and can be used for samples with sulphate concentration greater than 10 mg/L
(samples can be diluted and then it can be analysed).
SO42- + BaCl2  BaSO4
The absorbance of the barium sulphates formed is measured by a spectrophotometer at 420 nm and the
sulphates ion concentration is determined by comparison of the reading with a standard curve.
Materials Required
Apparatus Required
1. Whatman No. 1 filter paper
2. Spectrophotometer
3. Magnetic stirrer
4. Tissue Paper
Chemicals Required
1. Conditioning agent
2. Barium chloride
3. Standard sulphate solution
4. Distilled water
Procedure
PREPARATION OF REAGENTS
Conditioning reagent
• Measure exactly 25 ml glycerol and pour it to a dry clean beaker.
• Then, measure 15 mL of concentrated hydrochloric acid and add it to the same beaker.
• To the same beaker, add exactly 50 mL of 95 % isopropyl alcohol and mix well.
• Accurate weigh 37.5 g sodium chloride and dissolve it in distilled water.
• Then mix all the contents and make up the final volume to 250 mL using distilled water.
Standard sulphate solution
• Weigh accurately 1.479 g anhydrous sodium sulphate and dissolve it in distilled water.
• Take 1000 mL standard measuring flask and place a funnel over it.
• Transfer it to the 1000 mL standard flask and make up to 1000 mL using distilled water.
• (1 mL = 1.0 mg SO4
Preparation of Blank, Standards and sample for Testing
• Take six 50 mL glass stoppered standard flask (four for standards, one for the sample and one for the
blank).
• Add 10 mL of the standard sulphate solution to the first standard flask, 20 mL to the second, 30 mL to
the third and 40 mL to the fourth.
• To the fifth standard flask add 20 mL of the sample water.
• The sixth standard flask is for the blank, to this standard flask add distilled water alone.
• Add 5 mL of conditioning reagent to all the standard flasks.
• Then make up the volume to the 100 mL mark using distilled water.
Testing of Sample
• Filter the sample though filter paper (Whatman No. 1) and take 50 mL of filtrate in an Erlenmeyer flask.
• Add 20 mL buffer solution and mix in stirring apparatus. While stirring, add 0.15 g of barium chloride
to the sample and stir the sample with the help of magnetic stirrer for about an hour.
• Measure the absorbance against a distilled water blank (DO NOT ADD BARIUM CHLORIDE TO IT.) at
420 nm using spectrophotometer. Absorbance for the blank sample is taken to correct for sample
colour and turbidity.

DEPARTMENT OF CIVIL ENGINEERING, SNIT ADOOR

 EXPT NO. 3 CHLORIDES AND SULPHATES

• Process the standard solution of different strengths in similar way and record the absorbance for each
solution. Plot a standard sulphate calibration curve on a graph paper from these absorbance values
putting strengths (mg/L) on X-axis and absorbance @ 420 nm on Y-axis. Fit a best-fit linear model to
the data.
• Using the standard sulphate calibration curve (a linear-model; Equation EQUATION), find out sulphate
concentration in the given unknown sample in mg/L.
Observations

SAMPLE VOLUME OF THE SAMPLE/ ABSORBANCE

No. STANDARD (mL)
BLANK
STD 1
STD 2
STD 3
STD 5
1
2
3
Calculations
From the calibration Graph,
Y= mX+C
Where, Y = Absorbance of the sample
m = Slope of the straight line
X = Concentration of sulphate in mg
(𝑋)𝑋1000
Concentration of Sulphate in mg/L 𝑚𝐿 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
=
Results
The sulphate concentration of the given sample in mg/L=
Inference
Water containing high levels of sulphates, particularly magnesium sulphate and sodium sulphate may have a
laxative effect on persons using the water for the first time. These effects vary with the persons and appear to
last only until the person becomes accustomed to using the water. High sulphates content also affects the
taste of water and will form a hard scale in boilers and heat exchangers. For these reasons the upper
recommended limit for sulphates in water is 200 mg/L as per BIS. The given sample is having sulphate content
is ___ than 200mg/L, so it is/not fit for drinking.

DEPARTMENT OF CIVIL ENGINEERING, SNIT ADOOR