CHLORIDES

Chloride is a salt compound resulting from the combination of the gas chlorine and a
metal. Chlorine alone as Cl2 is highly toxic and it is often used as a disinfectant. In combination
with a metal such as sodium, it becomes essential for life.
Chloride can corrode metals and affect the taste of food products. Therefore, water is
used in industry or processed for any use has a recommended maximum chloride level. Chloride
can contaminate fresh water streams and lakes. Fish and aquatic communities cannot survive in
high levels of chlorides.
Almost all natural waters contain chloride and sulphate ions. Their concentrations vary
considerably according to the mineral content of the earth in any given area. In small amounts,
they are not significant. In large concentrations they present problems. Usually chloride
concentrations are low. Sulphates can be more troublesome because they generally occur in
greater concentrations. Low to moderate concentrations of both chloride and sulphate ions add
palatability to water. In fact, they are desirable for this reason. Excessive concentrations of either,
of course, can make water unpleasant to drink.
Reverse Osmosis will remove 90 95% of the chlorides because of its salt rejection
capabilities. Electrodialysis and distillation are two more processes that can be used to reduce the
chloride content of water. Strong base anion exchanger which is the later portion of a two-
column deionizer does an excellent job at removing chlorides for industrial applications.

PRINCIPLE:
Silver Nitrate reacts with chloride to form very slightly soluble white precipitate of AgCl.
At the end point, when all the chlorides get precipitated, free silver ions react with chromate to
form silver chromate of reddish brown colour.
REAGENTS:
1. 0.02 N Silver Nitrate Solution
2. Potassium Chromate, 5%
PROCEDURE:
Take 50ml of sample in a conical flask and add 2ml of potassium chromate
solution.
Titrate the contents against 0.02N silver nitrate solution until a persistent red tinge
appears.
CALCULATION:
Amount of Chloride present in the given sample, mg/L
= ml of AgNO3 consumed 1000 0.5
ml of sample taken

1
 TOTAL ALKALINITY

PRINCIPLE:
Total Alkalinity is a measure of capacity of the water to neutralize a strong acid. The
Alkalinity in the waters is generally imparted by the salts of carbonates, bicarbonates,
phosphates, nitrates, borates, silicates etc., together with the hydroxyl ion in the free state.
However, most of the waters are rich in carbonates and bicarbonates with little concentration of
other alkalinity imparting ions.
Total Alkalinity, carbonates, bicarbonates can be estimated by titrating the sample with a
strong acid (HCl or H2SO4), first to pH 8.3 using phenolphthalein as an indicator and then further
to pH between 4.2 and 5.4 with methyl orange or mixed indicator. In first case, the value is called
phenolphthalein alkalinity (PA) and in second case, it is total alkalinity (TA). Values of
carbonates, bicarbonates and hydroxyl ion can be computed from these two types of alkalinities.
REAGENTS:
1. 0.02N HCl
2. Phenolphthalein indicator
3. Methyl orange indicator
PROCEDURE:
Take 50ml of sample in a conical flask and add 2 drops of Phenolphthalein indicator.
If the solution remain colourless, P=0 and total alkalinity is prescribed as step 4.
If the colour changes to pink after addition of phenolphthalein, titrate it with 0.02N HCl
until the colour disappears at the end point. This is phenolphthalein alkalinity.
Now add 2 3 drops of methyl orange to the same sample and continue the titration
further, until the yellow colour changes to pink at the end point. This is total alkalinity.
CALCULATION:
Phenolphthalein Alkalinity as CaCO3, mg/L = A Normality of HCl 1000
ml of sample taken

Total Alkalinity as CaCO3, mg/L = B Normality of HCl 1000

ml of sample taken

Where,
A = ml of HCl used with only phenolphthalein.

B = ml of total HCl used with phenolphthalein and methyl orange.

TOTAL HARDNESS

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 Hard water results when an excessive amount of calcium and magnesium are present.
Total hardness is measured in milligram per litre (mg/L).
Hardness is measure of polyvalent cations (ions with a charge greater than +1) in
water. Hardness generally represents the concentration of calcium (Ca 2+) and magnesium (mg2+)
ions, because these are most common polyvalent cations. Other ions such as (Fe 2+) and
manganese (Mn2+), may also contribute to the hardness of water, but are generally present in
much lower concentrations. Waters with high hardness value are referred to as hard while
those with low hardness values are soft.

PRINCIPLE:
EDTA Method:
Hardness is generally caused by the calcium and magnesium ions present in water.
Polyvalent ions of some other metals like strontium, iron, aluminium, zinc and manganese etc.,
are also capable of precipitating the soap and thus contributing to the hardness. However, the
concentration of these ions is very low in natural waters. Therefore, hardness is generally
measured as concentration of only calcium and magnesium (as calcium carbonate), which are far
higher in quantities over other hardness producing ions.
Calcium and magnesium form a complex of wine red colour with Eriochrome Black T
indicator at pH of 10.0+ 0.1. The EDTA has got a stronger affinity towards Ca++ and Mg++ and
therefore, by addition of EDTA, the former complex is broken down and a new complex of blue
colour is formed.

REAGENTS:
1. 0.01N EDTA solution
2. Buffer solution
3. Eriochrome Black T indicator

PROCEDURE:
Take 50ml of sample in a conical flask. If the sample is having higher calcium, take a
smaller volume and dilute to 50ml using distilled water.
Add 1ml of buffer solution.
Add a small pinch of Eriochrome black T indicator, the solution turns wine red.
Titrate the contents against 0.01N EDTA solution. At the end point, colour changes from
wine red to blue.

CALCULATION:

Hardness as CaCO3, mg/L = ml of EDTA used 1000

ml of sample taken
DISSOLVED OXYGEN

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 Dissolved Oxygen (DO) is found in microscopic bubbles of oxygen that are mixed in the
water and occur between water molecules. DO is a very important indicator of a water bodys
ability to support aquatic life. Fish breathe by absorbing dissolved oxygen through their gills.
Oxygen enters the water by absorption directly from the atmosphere or by aquatic plant and
algae photosynthesis. Oxygen is removed from the water by respiration and decomposition of
organic matter.
PRINCIPLE:
WINKLERS IODOMETRIC METHOD:
The manganous sulphate reacts with the alkali (KOH or NaOH) to form a white
precipitate of manganous hydroxide which in the presence of oxygen, gets oxidized to a brown
colour compound. In the strong acid medium, manganic ions reduced by iodide ions which get
converted into iodine equivalent to the original concentration of oxygen in the sample. The
iodine can be titrated against thiosulphate using starch as an indicator.
REAGENTS:
1. 0.025N Sodium thiosulphate solution
2. Alkaline potassium iodide solution
3. Manganous sulphate solution
4. Starch solution
5. Concentrated Sulphuric acid
PROCEDURE:
Fill in the sample in a glass stoppered BOD bottle of known volume (300ml)
carefully, avoiding any kind of bubbling and trapping of the air bubbles in the
bottle after placing the stopper.
Pour 2ml of each manganous sulphate and potassium iodide solutions well below
the surface from the walls. Use always, separate measuring jar for these two
reagents. A precipitate will appear.
Place the stopper and shake the contents well by inverting the bottle repeatedly.
Keep the bottle for sometime to settle down the precipitate.
Add 2ml of concentrated H2SO4 along the sides and shake well to dissolve the
precipitate.
Take 203ml of the above content in a conical flask for titration. Prevent the
bubbling to avoid further mixing of oxygen.
Titrate the content against Sodium thiosulphate solution and starch as an indicator.
At the end point, initial dark blue colour changes to colourless.
CALCULATION:
203ml of the content for titrations contains 200ml of original sample.
1ml of 0.025N sodium thiosulphate = 0.2 mg of oxygen
ml of titrant = (ml of titrant 0.2mg of oxygen) / 200ml of sample
Dissolved Oxygen in the sample (mg/L) = ml of titrant 0.2 5
= ml of titrant.

CHEMICAL OXYGEN DEMAND (COD)

4
 Chemical oxygen demand is the oxygen demand required by the organic substances in
water to oxidise them by a strong chemical oxidant. The determination of COD values are of
great importance where BOD values cannot be determined very accurately due to the presence of
toxins and other such unfavourable conditions for growth of micro organisms. The main
disadvantage of this that oxygen is also consumed by the oxidation of inorganic matter such as
nitrites, sulphides, reduced metal ions. Thiosulphate and some other organic matters are not
oxidized by dichromate method such as benzene, pyridine and few other cyclic organic
compounds. Consequently, the test is a poor measure of strength of organic wastes unless these
factors are taken into consideration.
The COD test given no indication of whether or not the waste is biologically degradable
and nor does it indicate the rate at which biological oxidation would proceed and hence the rate
at which the oxygen would be required in a biological system.
Despite all these limitations, the COD test continues to remain a very important
parameter in management and design of the treatment plants because of its rapidly in
determination. COD values cannot be corresponded with that of BOD values. In general, COD is
more than the BOD values for most of the industrial wastes.

PRINCIPLE:
Chemical Oxygen Demand (COD) is a measure of oxygen consumed during the
oxidation of the oxidisable organic matter by a strong oxidizing agent. Potassium dichromate in
the presence of sulphuric acid is generally used as an oxidizing agent in determination of COD.
The sample is refluxed with K2Cr2O7 and H2SO4 in presence of mercuric sulphate to
neutralize the effect of chlorides and silver sulphate (catalyst). The excess of potassium
dichromate is titrated against ferrous ammonium sulphate using ferroin as an indicator. The
amount of K2Cr2O7 used is proportional to the oxidisable organic matter present in the sample.

REAGENTS:
1. 0.25N Potassium dichromate solution
2. 0.025N Potassium dichromate solution
3. 0.1N Ferrous Ammonium Sulphate solution
4. 0.01N Ferrous Ammonium Sulphate solution
5. Concentrated Sulphuric acid
6. Mercuric Sulphate
7. Ferroin Indicator

PROCEDURE:
Take 20ml of sample in a 250 500ml COD flask.

5
 If the sample is expected to have COD more than 50mg/L, add 10ml of 0.25N
Potassium dichromate solution. (In case, the COD is expected below 50mg/L, add
10ml of 0.025N Potassium dichromate solution).
Add a pinch of Ag2SO4 and HgSO4. If the sample contains chlorides a higher
amount, HgSO4 is added in the ratio 0f 10:1 to the chlorides.
Add 30ml of Sulphuric acid.
Reflux atleast for 2 hours on a water bath or a hot plate. Remove the flask, cool
and add distilled water to make final volume to about 140ml.
Add 2 3 drops of ferroin indicator mix thoroughly and titrate with 0.1N Ferrous
Ammonium Sulphate. (0.01N Ferrous Ammonium Sulphate is used if 0.025Nof
K2Cr2O7 is used).
Run a blank with distilled water using same quantity of chemicals.

CALCULATION:

COD, mg/L = (b-a) N of Ferrous Ammonium Sulphate 1000 8

ml of sample

BIO-CHEMICAL OXYGEN DEMAND (BOD)

BOD is the amount of oxygen utilized by micro-organisms in stabilizing the organic

matter. On an average basis, the demand for oxygen is proportional to the amount of organic
waste to be degraded aerobically. Hence, BOD approximates the amount of oxygen oxidisable

6
organic matter present in the soil solution and the BOD value can be used as measure of waste
strength. It is highly important to know the amount of organic matter present in the waste
treatment system and that the quantity of oxygen required for stabilization. The BOD values are
thus is very useful in the process design and loading calculations as well as the measure of
treatment plant efficiency and operation. The BOD is also useful in stream pollution control
management and in evaluating the self purification capacities of the streams which serves as the
measure to access the quantity of waste which can be safely assimilated by the stream.
The complete degradation of organic matter may take 20 to 30 days. Simple organic
compounds like glucose are almost completely oxidized in 5 days, while domestic sewage by
only about 65% and complex organic compounds might be oxidized only upto 40% in this
period. The 20 to 30 days period is of less significance. In practice, therefore the BOD has been
developed for 5 days at 20 degree centigrade.
Types of micro-organisms, pH and presence of toxins, some reduced mineral matter and
vitrification process are the important factors influencing the BOD test.

PRINCIPLE:
Bio-chemical Oxygen Demand (BOD) is the measure of degradable organic matter
present in water sample and can be defined as the amount of oxygen required by the micro-
organisms in stabilizing the biologically degradable organic matter under aerobic conditions. The
principle of the method involves measuring the difference of the oxygen concentration between
the sample and after incubating it for 5 days at 20 degree centigrade.

REAGENTS:
1. Phosphate buffer
2. Magnesium sulphate
3. Calcium chloride
4. Ferric chloride
5. Sodium sulphite solution

PROCEDURE:
Prepare dilution water in glass container bubbling compressed air in distilled
water for about 30 minutes.
Add 1ml each of phosphate buffer, magnesium sulphate, calcium chloride and
ferric chloride solutions for each litre of dilution water and mix thoroughly.
Neutralize the sample to pH around 7.0 by using NaOH or H2SO4.
Since the DO in the sample is likely to be exhausted, it is usually necessary to
prepare a suitable dilution of the sample according to the expected BOD
range.
Prepare dilution in a bucket or a large glass trough, mix the contents
thoroughly. Fill 2 sets of BOD bottles.

7
 Keep one set of the bottles in BOD incubator at 20 degree centigrade for 5
days and determine the DO in another set immediately.
Determine the DO in the sample bottles, immediately after completion of 5
days of incubation.
Similarly for blank, take 2 BOD bottles for dilution water. In one, determine
the DO content and the other incubate with the sample to determine DO after
5 days.

CALCULATION:
BOD, mg/L = [D0 D5] Dilution factor

D0 = Initial DO in the sample.

D5 = DO after 5 days.

OIL AND GREASES IN WASTEWATER

Oil and Grease is any material recovered as a substance soluble in petroleum ether,
Hexane or trichlorotrifluoroethane. It includes other material extracted by the solvent from an
acidified sample such as sulphur compounds, certain organic dyes and chlorophyll and non
volatilized during the test.

8
 The Oil and Grease content of domestic and certain industrial wastes and of sludge is an
important consideration in the handling and treatment of these materials for ultimate disposal.
Certain constituents measured by the Oil and Grease analysis may influence wastewater
treatment systems. If present is excessive amount, they may interference with aerobic and
anaerobic biological processes and lead to decreased wastewater treatment efficiency. When
discharged in wastewater or treated an effluent leads to environmental degradation.
A Known Oil is defined as a sample of oil and or grease that represents the only
material of that type used or manufactured in the processes represented by a wastewater.
Unknown Oil is defined as one for which a representative sample of the oil or grease is not
available for preparation of a standard. The term grease grease applies to a wide organic
substance that is extracted from aqueous solution or suspension by hexane. Hydrocarbons, esters,
oils, fats, waxes and high molecular weight fatty acids are the major materials dissolved by
hexane. All these materials have a Greasy feel and are associated with the problems in
wastewater treatment related to grease. (Hexane has been selected for the solvent in grease
determinations because it is a good solvent for all material normally associated with the term
grease and has a minimum solvent for other organic compounds).

PRINCIPLE:
Oil and Grease present in the water can be extracted in petroleum ether, which is
immiscible in water and can be separated by a separating funnel. The residue, after evaporation
of this petroleum ether will yield the oil and grease.
Samples for determination of oil and grease should be collected in a wide mouth glass
bottle separately and it is preferable to use the entire sample, without subdivision for analysis.
For preservation of the sample acidify with H2SO4 never use chloroform as a preservative.

APPARATUS AND REAGENTS:

1. Separating Funnel, 500ml

2. Water bath
3. Filter paper
4. H2SO4 (1:2)
5. Petroleum Ether

PROCEDURE:

Take 200 250ml of sample in a separating funnel.

Add 10ml of H2SO4 (1:2) and 50 ml of Petroleum ether to the sample.
Shake well and if suspension prevails, add small amount of ethyl alcohol. Keep
for sometime for separation of the two layers. The upper one is petroleum ether
with oil and grease and the lower one is the sample.

9
 Discard lower layer of the sample through separating funnel.
Take a pre-weighed dish or a small beaker and run into it, the petroleum ether
from the separating funnel through a filter paper which has already been moisten
with fresh petroleum ether.
Evaporate the petroleum ether on a water bath and take the final weight of the
dish or the beaker after cooling in a dessicator. Never heat petroleum ether on a
flame.

CALCULATION:

Oil and grease in mg/L = (A-B) 1000 1000

V
Where,
A = Final weight of dish in g
B = initial weight of dish in g
V = Volume of sample taken in ml.

OPTIMUM COAGULANT DOSAGE

COAGULATION:
In traditional water system, certain chemicals are added to raw water to remove
impurities. While some particles will spontaneously settle out from water on standing (a process
called sedimentation), others will not. To cause particles that are slow to settle or non-settling to
settle out more readily, a soluble chemical or mixture of chemicals is added to the water. Such a
chemical is called a coagulant and the process is called coagulation. The coagulant reacts with

10
the particles in the water, forming large particles called flocs, which settle rapidly. Flocs can also
be effectively removed by passing the water through a filter. The process is controlled so that the
coagulant chemicals are removed along with the contaminants. Coagulation/ Flocculation
processes generally use aluminium sulphate (alum) or ferric chloride as the coagulant. A
combination of coagulation/ flocculation/ sedimentation and filtration is the most widely applied
water treatment technology around the world, used routinely for water treatment since the early
part of the 20th century.
Coagulation/ flocculation processes are very effective for removing fine suspended
particles that attract and hold bacteria & viruses to their surface. Research has shown that these
processes alone are capable of removing up to 99.9% of the bacteria and 99% of the viruses from
water supplies.
These processes also remove some of the organic matter washed from soil and vegetation
as water travels across the landscape, from raindrop to river. It is usually this natural organic
matter that is responsible for any brown discolouration in water. However, not all of this natural
organic matter is removed by coagulation: certain taste and odour problems may remain.
Coagulation processes is an important part of water and wastewater treatment.
Coagulation or destabilization of a colloidal suspension results in joining of minute particles by
physical and chemical processes. Flocculation results in formation of a large settleable structure
by bridging. These processes commonly used to remove suspended matter or colour. Adsorption
of ionic forms also occurs to varying degrees depending on the constituents in the water or
wastewater.
The jar test is a laboratory technique for determining the most effective coagulant,
chemical dose and operating pH for coagulation and flocculation, aluminium or iron salts may be
used to coagulate particles and to form settleable flocs composed of the hydrous metal oxide
precipitates and impurities.
Coagulation and flocculation experiments may also be used in conjunction with other
tests to study basic processes including, for example, the kinetics of reaction and the removal of
trace constituents from aqueous solution.

PRINCIPLE:
Coagulation is not an exact science although recent advances have been made in
understanding the process mechanics. Therefore, selection and optimum coagulant dosages are
determined experimentally by jar test instead of quantitatively by formula. The jar test must be
performed on water that is to be coagulated and must be repeated with each significant change in
the quality of given water.

REAGENTS AND APPARATUS:

1. Jar test apparatus
11
 2. Standard Coagulant solution
3. Stop watch
4. Beaker

PROCEDURE:
Jar test apparatus consists of six jars with stirring device that simultaneously
mixes the contents of each jar with a uniform power input. Each of the six jars is
filled with water whose optimum coagulant dosage is to be determined up to the
one litre mark.
Each jar is dosed with different amounts of coagulant with the help of standard
coagulant solution.
After coagulant dosing, water is mixed rapidly for 1 minute to ensure complete
dispersion of the chemicals, then mixed slowly for 15 to 20 minutes to aid in the
formation of flocs.
Allow the sample to stand for 30 minutes, then pipette out suspended liquid into
clean containers very carefully.
Analyse the above pipette out sample using turbidity meter.
Plot the graph between turbidity Vs coagulant dosages. From the graph, optimum
coagulant dosage could be determined.

RESULT:
Optimum coagulant dosage of ferric chloride coagulant for the given sample is ________

SULPHATES

Sulphate is a substance that occurs naturally in drinking water. Health concerns regarding
sulphate in drinking water have been raised because of reports that diarrhoea may be associated
with the ingestion of water containing high levels of sulphate. Of particular concerns are group
within the general population that may be at greater risk from the laxative effects of sulphate
when they experience an abrupt change from drinking water with low sulphate concentrations to
drinking water with high sulphate concentrations. Ion exchange is the most known method of
eliminating big quantities of sulphate from water for public, livestock and commercial supplies.

12
But, it is not used for individual household water treatment. It is a process where one element or
chemical is replaced for another.

PRINCIPLE:
Sulphate ion is precipitated in the form of barium sulphate by adding barium chloride in
hydrochloric acid medium. The concentration of sulphate can be determined from the absorbance
of the light by barium sulphate and then comparing it with a standard curve.
Suspended matter and original colour of the sample may interference with the sulphate
determination. Suspended matter can be removed by filtration. Presence of silica in excess of
500mg/L and large quantity of organic matter may affect the satisfactory precipitation of barium
sulphate.
APPARATUS AND REAGENTS:
1. Stock Sulphate solution
2. Conditioning reagent
3. Barium Chloride crystals
4. Magnetic Stirrer
5. Spectrophotometer

PROCEDURE:
Take 100ml of sample (not containing more than 40mg/L of SO 4) or a suitable
aliquot diluted to 100ml in 250ml conical flask.
To this, add 5ml of conditioning reagent.
Stir the sample on a magnetic stirrer and during stirring, add a spoonful of BaCl 2
crystals. Stir for only one minute after addition of BaCl2 crystals.
Take the reading on a spectrophotometer at 420nm exactly after 4 minutes. Find
out the concentration of sulphate from the standard curve.
Prepare the standard curve, employing the same procedure as described above, for
0.0 40.0 mg/L at the interval of 5mg/L.

RESULT:
The amount of Sulphates present in the given samples is ______________
FLUORIDES

Fluoride ions have dual significance in water supplies. High concentration of fluoride
causes dental fluorisis (Disfigurement of the teeth). At the same time, a concentration less than
0.8 mg/L results in Dental caries. Hence, it is essential to maintain the fluoride concentration
between 0.8 to 1.0 mg/L in drinking water. On the other hand, some children under nine years of
age exposed to levels of fluoride greater than about 2mg/L may develop a condition known as
endemic dental fluorisis. Sometimes called Colorado Brown Stain, this condition appears as
a dark brown mottling or spotting of the permanent teeth. In certain cases, the teeth become
chalky white in appearance. Further, federal regulations require that fluoride not exceed a

13
concentration of 4 mg/L in drinking water. This is an enforceable maximum contaminant level
standard and it has been established to protect public health. Exposure to drinking water levels
above 4 mg/L for many years result in cases of crippling skeletal fluorisis, which is a serious
bone disorder.
Research studies indicate that fluoride concentrations of 1 mg/L are optimum. Authorities
generally agree: (i) where concentrations are greater than 4 mg/L, the excess fluorides must be
removed from water. (ii) where concentrations are less than 1 mg/L, fluorides should be added.
As a result of studies, cities are presently required by some states to add fluorides in optimum
concentrations to municipal water supplies. (iii) where the fluorides concentration is too great, it
is necessary to reduce the amount to acceptable limits.

PRINCIPLE:
Fluoride ion changes the colour of Zirconium SPANDNS complex and the colour
change is proportional to the fluoride ion concentration.

APPARATUS AND REAGENTS:

1. Fluoride Stock solution
2. Acid Zirconyl SPADNS reagent
3. Spectrophotometer
PROCEDURE:
Take 50ml of sample or a suitable aliquot diluted to 50ml in 100ml conical flask.
To this, add 10ml of acid zirconyl SPADNS reagent.
Take the reading on a spectrophotometer at 570nm as soon. Find out the
concentration of fluorides from the standard curve.
Prepare the standard curve of fluorides in the range of 0.2 to1.60 mg/L by diluting
the appropriate volume of stock fluoride solution to 50ml in a 100ml conical flask
and employing the same procedure as described earlier.

RESULT:
The amount of Fluorides present in the given samples is ______________
NITRATES

Nitrates are a nitrogen/oxygen compound that naturally occurs in low concentrations in

ground water. Under normal circumstances, only a very small percentage of the total nitrates
consumed by adults come from drinking water. The vast majority of nitrates in the diet normally
come from cured meats and vegetables such as spinach, lettuce, beets and carrots. Nitrates are
derived from nitrogen an element which occurs naturally in many different forms in the
environment. When nitrogen enters the soil, it is converted to nitrates by micro-organisms. Plants
use some of these nitrates; any excess is carried down through the soil into the groundwater in a
process known as leaching.
At times, far more nitrogen enters the soil than plants can use leading to dangerously high
levels in groundwater. Animals and human waste contains nitrogen in the form of ammonia.

14
Runoff from agricultural lands can also cause elevated nitrate levels, because fertilizer contains a
lot of nitrogen. Decomposing plant and animal material can also generate nitrates. Most cases of
nitrates contamination occur in agricultural areas. In fact, concentrations of 30 milligrams a litre
or higher can occur in some cases.
Drinking water quality standards have been set to offer the greatest protection to infants.
The standard of 45 milligrams nitrate (NO 3) has a small margin of safety built into it. Because of
this safety factor, some adults can drink water exceeding the standard and show no adverse
effects. However, high nitrate levels are usually an indication of surface water contamination of
the water supply. Nitrate levels exceeding the standard are a warning of other water quality
problems.
Because nitrate is tasteless and odourless, water must be chemically tested to determine if
it is contaminated. If you are on a municipal or public water system, it is responsibility of the
water authority to test and treat the water supply to prevent nitrate contamination. If nitrate
contamination occurs in a public water supply, customers may be warned not to feed the water to
infants until the problem is corrected. However, if you are on a private or individual water
system, it is your responsibility to monitor for nitrate.
Nitrate is a very soluble substance, easily dissolved in water and extremely hard to
remove it. Treatment for nitrate is very complicated and expensive. However, only water used for
drinking and cooking needs to be treated. The method of reducing or removing nitrate is (i)
demineralization by distillation or reverse osmosis (ii) ion exchange.

PRINCIPLE:
Nitrate ion reacts with brucine in strong sulphuric acid solution to form a yellow colour
which is measured spectrophotometrically.

INTERFERENCES:
All strong oxidizing and reducing agents interfere. Chlorine interference upto 5 mg/L is
eliminated by the addition of arsenite. Ferrous iron, ferric ion and tetravalent manganese
interfere when present in concentration more than 1 mg/L. The interference by nitrite upto 5
mg/L is eliminated by the use of sulphanilic acid. High content of organic matter may also
interfere.

REAGENTS:
1. Nitrate Stock solution
2. Nitrate Standard solution
3. Brucine Sulphanilic acid solution
4. Sulphuric acid solution

PROCEDURE:
In to a series of 50ml conical flask pipette out 1ml, 2ml, 3ml, 4ml and 5ml of
standard nitrate solution and dilute each to 5ml with distilled water. Include a
conical flask containing 5ml distilled water as the blank.

15
 Place 2ml or suitable aliquot of the sample (not exceeding 5ml) containing not
more than 10mg/L nitrate nitrogen in a 50ml conical flask and dilute the
volume to 5ml. If the sample contains any residual chlorine, add 0.1 ml sodium
arsenite solution to a 50ml portion of the sample for each 0.05mg/L chlorine.
Add one drop in excess and mix well. Take aliquots of this arsenite treated
sample for nitrate nitrogen determination.
Add 1ml of brucine sulphanilic acid solution to blank, standards & sample
and mix well.
Transfer the contents of the series of 50ml conical flask containing blank,
standards and sample to each of second series of 50ml conical flask containing
sulphuric acid solution and mix well. Pour from one conical flask to the other
three or four times to ensure complete mixing.
Keep the conical flask in the dark for 10 minutes.
While the colour is developing, measure 10ml distilled water to other set of
empty conical flask. After 10 minutes add the distilled water in the respective
conical flask containing blank, standards and sample.
Allow to cool in the dark for 20 to 30 minutes.
Measure the absorbance of the standards and the sample after setting the blank
at 100% transmittance at a wavelength of 410nm. If spectrometer is not
available, use a filter photometer equipped with a violet filter having a
maximum transmittance between 400 and 425mm.
Prepare a calibration curve and find out the mg equivalent of nitrate nitrogen in
the sample. Express the result as mg nitrate nitrogen per litre of the sample.

CALCULATION:

mg/L nitrate nitrogen N = mg Nitrate Nitrogen 1000

ml of sample taken for estimation

mg/L NO3 = mg/L Nitrate Nitrogen 4.43

RESIDUAL CHLORINE

Water used for drinking and cooking should be free of pathogenic (disease causing)
microorganisms that cause such illnesses as typhoid fever, dysentery, cholera, and gastroenteritis.
Whether a person contracts these diseases from water depends on the type of pathogen, the
number of organisms in the water (density), the strength of the organism (virulence), the volume
of water ingested, and the susceptibility of the individual. Purification of drinking water
containing pathogenic microorganisms requires specific treatment called disinfection. Although
several methods eliminate disease-causing microorganisms in water, chlorination is the most

16
commonly used. Chlorination is effective against many pathogenic bacteria, but at normal
dosage rates it does not kill all viruses, cysts, or worms. When combined with filtration,
chlorination is an excellent way to disinfect drinking water supplies.

Tests for chlorine residual are probably the most frequently performed tests at water
treatment plants. The word "residual" means "remainder" or "that which is left", and as the name
suggests the chlorine residual test is used to measure the amount of chlorine remaining in the
water at the time the test is made. The chlorine residual is usually tested in finished water which
is ready to be released into the distribution system, although operators must also ensure that there
is adequate residual at the extreme ends of the distribution system.

Chlorine readily combines with chemicals dissolved in water, microorganisms, small

animals, plant material, tastes, odours and colours. These components "use up" chlorine and
comprise the chlorine demand of the treatment system. It is important to add sufficient chlorine
to the water to meet the chlorine demand and provide residual disinfection.

The chlorine that does not combine with other components in the water is free (residual)
chlorine, and the breakpoint is the point at which free chlorine is available for continuous
disinfection. An ideal system supplies free chlorine at a concentration of 0.3-0.5 mg/l. Simple
test kits, most commonly the DPD colorimetric test kit (so called because diethyl phenylene
diamine produces the color reaction), are available for testing breakpoint and chlorine residual in
private systems. The kit must test free chlorine, not total chlorine.

PRINCIPLE:

Free Chlorine reacts with DPD to form a red-violet compound. By comparing the colour
against a set of reference standards, the amount of free residual chlorine can be determined.

REAGENTS AND APPARATUS:

1. Chlorine solution
2. Lovibond Colour Comparator
3. DPD Tablet
PROCEDURE:

Take 100 ml of water sample in five numbers of conical flasks. To this, add 0.1,
0.2, 0.3, 0.4 and 0.5 ml of chlorine solution and kept aside for 20 minutes for
complete reaction.
After 20 minutes, add one number DPD tablet to a few ml of the water sample in
the 10ml comparator tube provided.

17
 Using a clean rod, crush the tablet in the water sample or wait 1 2 minutes for
the tablet to dissolve naturally.
Fill the tube to the 10ml mark with the water sample and mix DPD tablet
thoroughly. Place the tube in the right hand compartment of the comparator.
Fill another comparator tube to the 10ml mark with the water sample (without
DPD tablet) and place this in the left hand compartment of the comparator.

Now the comparator disc is rotated till the colours match. The comparator discs
will be available in two different chlorine concentration ranges; 0.1 to 1.0 mg/L of
chlorine and 0.2 to 4.0 mg/L of chlorine. The residual chlorine amount can be
directly read from the window in the lower right corner of the instrument.

Record the amount of free residual chlorine in mg/L in the sample.

When strong colour is obtained which subsequently fades or disappears altogether
when the solution is made upto full volume, this indicates that a high
concentration of chlorine is present. The water sample should be diluted and re
tested.

RESULT:

From the graph, Optimum Chlorine dosage for the given water sample is ___________

WATER SOFTENING USING LIME AND SODA

Lime-soda ash treatment for the reduction of hardness involves the addition of slake
lime [Ca(OH)2] to a hard water supply to remove the carbonate hardness by precipitation with

18
the precipitation being removed by filtration. Non-carbonate hardness is in turn reduced by the
addition of soda ash (Na2C03) to form insoluble precipitate which is also removed by filtration.

This particular method of removing hardness sometimes used by municipal water plants to
reduce the amount of calcium and magnesium in a water supply. While it is quite effective in
reducing hardness, it is not a complete removal treatment. Often when a city has a raw water
source that has 35 to 40 grain hard water, the local water system will use the lime-soda ash
treatment to reduce hardness to between 5 and 10 grains.

Lime-soda ash treatment becomes increasingly costly when the hardness of the water
must be reduced to less than 5 grains. Municipally, the complete elimination of hardness is rarely
attempted as less than 5% of a municipality's water is used for home consumption. The use of
soda ash for the reduction of non-carbonate hardness increases the sodium in the effluent water
in the same proportion as ion exchange softening.

The use of the lime-soda ash treatment is impractical for individual home softening of
supplies. For one thing, there are difficulties in feeding lime and soda ash into raw water. Further,
close control of the operation is required both while the settling and filtering occurs.

An additional deterrent to home use of the lime-soda ash treatment is the size of the equipment
necessary, together with the high cost of this method of treatment.

PRINCIPLE:

Lime-soda ash treatment is especially effective if water contains bicarbonate (temporary)

hardness. Where calcium and magnesium are primarily in chloride or sulfate compounds, this
treatment is noticeably less effective.

Slaked lime is used to remove calcium bicarbonate from water. In the water to be treated,
the slaked lime ions react with the calcium bicarbonate to form the very slightly soluble calcium
carbonate. This precipitated material is usually removed by first settling and then filtering.

Ca(OH) 2+ Ca(HC03)2 --> 2 CaCO3 + 2 H2O

Calcium hydroxide plus calcium bicarbonate reacts to form calcium carbonate plus water.

To remove the magnesium, additional lime is used. The reaction for this process is:

Ca(OH) 2 + Mg --> Mg(OH) 2 + Ca++

Note: The arrow pointing down () indicates the formation of an insoluble compound.

19
 Calcium hydroxide plus magnesium ions react to form magnesium hydroxide plus
calcium ions. This step has simply replaced the magnesium with calcium. If soda ash is then fed
into the water, the calcium will precipitate as calcium carbonate:

Ca++ + Na2CO3 --> CaCO3 + Na+

Calcium ions plus sodium carbonate react to form calcium carbonate plus sodium ions.

REAGENTS:

1. O.25N Calcium hydroxide solution

2. 0.25N Sodium carbonate solution

3. EDTA solution

4. Buffer solution

5. Eriochrome Black T Indicator

PROCEDURE:

Take 50ml of sample in a conical flask and add 1ml buffer solution and a pinch of
Eriochrome Black T Indicator to it and titrate it on against EDTA solution. This is
for to find the initial hardness of the given sample.

Then take 50ml of sample in five set of 250ml conical flask. To this, add calcium
hydroxide solution (lime) in different dosages such as 0.2ml, 0.4ml, 0.6ml, 0.8ml
& 1 ml and allowed to settle for one minute.

After that, filter the sample and collect the residue and follow the same procedure
as above (add 1ml buffer solution and a pinch of Eriochrome Black T Indicator to

20
 it and titrate it on against EDTA solution). Note down the reduction of hardness
level in the sample.

The dosage which gives minimum hardness was found and it is selected as an
optimum dosage for further reduction of hardness using sodium carbonate
solution (soda).

Then soda was added in varying dosages (0.1ml, 0.2ml and 0.3ml) for the next
three set of conical flask and follow the same procedure for the reduction of
hardness using lime as above.

Finally, the optimum dosage of the given sample is found and from this
percentage reduction of hardness is determined. Thus the water is softened using
lime and soda.

RESULT:

Optimum Lime dosage = ml/L

Optimum Soda dosage = ml/L

Sample hardness as CaCO3 = mg/L

Reduction of Hardness = mg/L

Percentage Reduction = %

DETERMINATION OF SODIUM AND POTASSIUM IN WATER

21
 Sodium is present in number of minerals, the principle one being rock salt (sodium
chloride). The increased pollution of surface and ground water during the past has resulted in a
substantial increase in the sodium content of drinking water in different regions of the world.
Sewage, industrial effluents, sea water intrusion in coastal area and the uses of sodium
compounds for corrosion control and water softening processes all contribute to sodium
concentration in water because of the high solubility of sodium salts and minerals. Sodium levels
in ground water vary widely but normally range between 6 and 130 mg/L. In surface water, the
sodium concentration may be less than 1 mg/L or exceed 300 mg/L depending upon the
geographical area. Seawater contains about 400 ppm potassium. It tends to settle, and
consequently ends up in sediment mostly. Rivers generally contains about 2-3 ppm potassium.
This difference is mainly caused by a large potassium concentration in oceanic basalts.

In general, sodium salts are not actually toxic substances because of the efficiency with
which mature kidneys excrete sodium. Excessive intake of sodium chloride causes vomiting and
the elimination of much by the sweat. The taste threshold of sodium in water depends upon the
associated anions and the temperature f the solution. Sodium Carbonate has the lowest taste
threshold and the bicarbonate salt is the highest. At room temperature, the various threshold
values for sodium were found to be about 20mg/L for Na 2CO3, 150 mg/L for NaCl, 190 mg/L for
NaNO3, 220 mg/L for Na2SO4 and 400 mg/L for NaHCO3. The recommended guideline value is
200 mg/L which is based above taste thresholds and on health consideration.

Potassium is the major intracellular cation. It is widely distributed in the body in muscle
tissue, nerve tissue, blood cells and plasma. It is filtered in the glomerulus, absorbed in the
proximal tubule and finally excreted by exchange for sodium in the distal tubule. Potassium
influences muscular activity, cardiac function and nerve conduction process. In hyperkalemia
the plasma potassium concentration exceeds 5.5 mmol/L. Acute hyperkalemia is a medical
emergency. In hypokalemia the plasma potassium level will be less than 3.5 mmol/L. This can
occur due to excessive loss in gastro-intestinal secretions and urine, and also in renal tubular
acidosis. Excessive sodium intake, especially when accompanied by inadequate potassium
intake, raises blood pressure (BP), a well-accepted and extraordinarily common risk factor for
stroke, coronary heart disease (CHD) and kidney disease.

INSTRUMENTATION:

FLAME PHOTOMETER:

Flame photometry is an atomic emission technique which may be regarded as the

simplest of atomic spectroscopic methods and is very similar to the flame test which is applied
for detection of alkali metals. Flame photometry is good only for elements that are easily excited

22
and do not require very high temperatures (Na, K, Li, Ca are the most widely determined atoms
by this technique).
A flame photometer instrument is extremely simple where the sample in solution is
aspirated through an aspirator or nebulizer into the flame which is usually a propane / air fuel or
a purified natural gas/air mixture. The sample matrix evaporates followed by atomization of the
sample. Atoms present in the high temperature zone of the flame are excited to higher energy
levels by absorbing energy from the flame. As excited atoms return to the ground state they emit
radiation in definite wavelength depending on the energy level from which each atom drop. This
gives rise to a line spectrum. However, in flame photometry a pre-selected filter is used and it is
the intensity of the emission line that is practically measured and is related to the original
concentration of the sample in solution. The detector is usually a phototube or a photomultiplier
tube depending on the quality of the instrument.

PRINCIPLE:
When a solution of an inorganic salt such as sodium chloride is sprayed into the
flame, the elements in the compound are partly converted into the atomic state. Due to the heat
energy of the flame a very small proportion of these atoms are excited and the electrons move to
a higher energy level. The proportion of the atoms that are excited depends upon the
concentration of the particular element and on the temperature of the flame. In the excited state
the electrons are unstable and they rapidly revert back to their former lower energy level. As they
change from the excited state or higher energy level back to the lower energy level, they emit the
light in the form of a fixed wavelength, to produce a spectrum. Under carefully controlled
conditions the amount of light emitted is directly proportional to the number of atoms that are
excited, which in turn is proportional to the concentration of the substance in the sample.

REAGENTS AND APPARATUS:

1. Sodium stock solution (1000mg/L)
2. Potassium stock solution (1000 mg/L)
3. Flame Photometer

PROCEDURE:
Prepare the standard solution of sodium and potassium at different concentration
(25mg/L, 50mg/L, 100mg/L and 200mg/L) from the given stock solution (1000
mg/L) in a 100ml beaker.
Follow instructions for the correct operation of the flame photometer available.
Start the electrical supply and switch on the air supply.
Also switch on the gas and maintain the gas fuel mixture so that the blue flame is
seen through the viewing window.
Aspirate distilled water and clean the nebulizer tube for every time to remove any
impurities present.
Calibrate the instrument by aspirating the standard to desire range.

23
 After that, place the unknown sample and note that, every time should be clean
the nebulizer tube with the distilled water is an important.
If the signal obtained for the sample is out of range, dilute a portion of the sample
properly till a signal within the range is obtained.
Construct a calibration curve for Na and K in the sample and measure the results
in ppm.
Thus the concentration of sodium and potassium in the given sample can be found
using flame photometrically.

RESULT:
1. The amount of sodium concentration present in the sample = _________ mg/L.

2. The amount of potassium concentration present in the sample = _________ mg/L.

24
 DETERMINATION OF IRON AND COPPER IN WATER

Toxic metals can be present in industrial, municipal and urban runoff, which can be
harmful to humans and aquatic life. Increased urbanization and industrialization are to blame for
an increased level of trace metals, especially heavy metals in our waterways. There are over 50
elements that can be classified as heavy metals, 17 of which are considered to be both very toxic
and relatively accessible. Toxicity levels depend on the type of metal, its biological role, and the
type of organisms that are exposed to it.
The heavy metals linked most often to human poisoning are lead, mercury, arsenic and
cadmium. Other heavy metals, including copper, zinc, iron and chromium, are actually required
by the body in small amounts, but can also be toxic in larger doses.
Heavy metals in the environment are caused by air emissions from coal-burning plants,
smelters, and other industrial facilities; waste incinerators; process wastes from mining and
industry; and lead in household plumbing and old house paints. Industry is not totally to blame,
as heavy metals can sometimes enter the environment through natural processes. For example, in
some parts of the U.S., naturally occurring geologic deposits of arsenic can dissolve into
groundwater, potentially resulting in unsafe levels of this heavy metal in drinking water supplies
in the area. Once released to the environment, metals can remain for decades or centuries,
increasing the likelihood of human exposure. In addition to drinking water, we can be exposed
to heavy metals through inhalation of air pollutants, exposure to contaminated soils or industrial
waste, or consumption of contaminated food. Because of contaminated water, food sources such
as vegetables, grains, fruits, fish and shellfish can also become contaminated by accumulating
metals from the very soil and water it grows from.

Iron ingestion is not generally unhealthy & is absolutely necessary in small amounts.
However, some research has found over exposure to iron, especially the addition of iron in water
can lead to heart disease, cancer & diabetes. The problem with iron is that it is often included in
supplements & enriched products. It is also in red meat & so it may be quite easy to consume too
much iron. If we add extra iron to the water supply, it is almost certain that consumers will be
ingesting too much iron with little difficulty.

Copper is an essential element to virtually all plants and animals, including humans.
Elevated levels of copper are toxic in aquatic environments and may adversely affect fish,
invertebrates, plants, and amphibians. Acute toxic effects may include mortality of organisms;
chronic toxicity can result in reductions in survival, reproduction, and growth.

In humans, small amounts of copper are necessary to maintain good health; however,
higher concentrations of copper may cause health effects such as irritation of the nose, mouth,

25
and eyes; nausea; and diarrhea. Some people who drink water containing copper in excess of the
action level may with short term exposure, experience gastrointestinal distress and with long-
term exposure may experience liver or kidney damage. People with Wilson's disease should
consult their personal doctor if the amount of copper in their water exceeds the action level.

INSTRUMENTATION:

ATOMIC ABSORPTION SPECTROPHOTOMETER:

The major components of atomic absorption spectrophotometer are a radiation source, the
flame, a monochromator and a detector circuited with a recorder. The source of radiation is
always a hollow cathode lamp. The radiation from this lamp enters the flame through a chopper
which sends the radiation intermittently.

Hollow Cathode Chopper Flame Monochromator Detector Recorder

Sample

An outline diagram underlying the principles and components of Atomic Absorption Spectrophotometer

Various kinds of flames such as acetylene-air, acetylene-oxygen, acetylene-nitrous oxide,

hydrogen-air, hydrogen-oxygen, and propane air are employed depending on the temperature
required for atomization of a particular element. The sample is aspirated into the flame through
the burner for atomization. The atomic vapours of the element absorb a portion of the radiation

26
and the remaining is transmitted to monochromator which selects only the required wavelength.
The monochromator is set on the wavelength emitted by hollow cathode lamp which is specific
to the element being estimated. The radiation after passing through the monochromator reaches
to a detector which produces an electrical signal. This signal is then amplified and displayed by
the recorder. The radiation produced by the flame itself is also reaching the detector, but the
amplifier is tuned to the frequency of the chopper so that only A.C radiation will be monitored.
The D.C radiation from the flame is automatically excluded. The chopper may be a mirror which
alternatively sends the radiation through the flame and directly (excluding the flame) to the
detector circuit. These types of instruments are called double beam AAS which measures I o/I. In
the single beam instruments, the radiation simply reaches intermittently through the flame and in
this case only I (transmitted radiation) is measured.

PRINCIPLE:

Atomic Absorption Spectroscopy is the determination of the presence and concentrations

of metals in liquid samples. Metals include Fe, Cu, Cr, Pb, Ni, Zn, Cd and many more. Typical
concentrations range in the low mg/L (ppm). Atomic absorption measures the amount of light at
the resonant wavelength which is absorbed as it passes through a cloud of atoms. As the number
of atoms in the light path increases, the amount of light absorbed increases in a predictable way.
By measuring the amount of light absorbed, a quantitative determination of the amount of
analyte element present can be made. In atomic absorption spectrophotometer, light of a specific
wavelength is passed through the atomic vapour of an element of interest and measurement is
made of the attenuation of the intensity of the light as a result of absorption.

Metals will absorb ultraviolet light in their elemental form when they are excited by heat,
either by flame or graphite furnace. Each metal has a characteristic wavelength that will be
absorbed. The AAS instrument looks for a particular metal by focusing a beam of UV light at a
specific wavelength through a flame and into a detector. The sample of interest is aspirated into
the flame. If that metal is present in the sample, it will absorb some of the light, thus reducing its
intensity. The instrument measures the change in intensity and converts the change in intensity
into an absorbance. As the concentration rises up, absorbance also rises up. Thus the calibration
curve can be detected by running standards of various concentrations on the AAS and observing
the absorbance. The ease and speed at which precise and accurate determinations can be made
with this technique have made atomic absorption is the one of most popular methods for the
determination of metals.

PROCEDURE:

Prepare the standard solution of iron and copper at varying concentration from the
given stock solution (1000 mg/L) in a 100ml beaker.

27
 Follow instructions for the correct operation of atomic absorption
spectrophotometer available.
Start the electrical supply and switch on the air supply.
Also switch on the gas and maintain the gas fuel mixture so that the blue flame is
seen through the viewing window.
Aspirate distilled water and clean the tube for every time to remove any
impurities present inside of the instrument.
Calibrate the instrument by aspirating the standard to desire range.
After that, place the unknown sample and note that, every time should be clean
the tube with the distilled water is an important.
If the signal obtained for the sample is out of range, dilute a portion of the sample
properly till a signal within the range is obtained.
Construct a calibration curve for iron and copper in the sample and measure the
results in ppm.
Thus the concentration of heavy metals present in the given sample can be
determined.
RESULT:
1. The amount of iron concentration present in the sample = _________ mg/L.

2. The amount of copper concentration present in the sample = _________ mg/L.

TOTAL SOLIDS

The term Total Solids refer to matter suspended or dissolved in water or wastewater
and is related to both specific conductance and turbidity. Total solids also referred to as total
residue is the term used for material left in a container after evaporation and drying of water
sample. Total solids include both total suspended solids, the portion of total solids retained by a
filter and total dissolved solids, the portion that passes through a filter.

Total solids are important to measure in areas where there are discharges from
sewage treatment plants, industrial plants, or extensive crop irrigation. In particular, streams and
rivers in arid regions where water is scarce and evaporation is high tend to have higher
concentrations of solids and are more readily affected by human introduction of solids from land
use activities.

Total solids measurements can be useful as an indicator of the effects of runoff from
construction, agricultural practices, logging activities, sewage treatment plant discharges, and
other sources. As with turbidity, concentrations often increase sharply during rainfall, especially
in developed watersheds. They can also rise sharply during dry weather if earth-disturbing
activities are occurring in or near the stream without erosion control practices in place. Regular
monitoring of total solids can help detect trends that might indicate increasing erosion in

28
developing watersheds. Total solids are related closely to stream flow and velocity and should be
correlated with these factors. Any change in total solids over time should be measured at the
same site at the same flow.

PRINCIPLE:

Solids are determined as the residue left after evaporation of the unfiltered sample.

APPARATUS:

1. Water bath

2. Dessicator

PROCEDURE:

Take an evaporating dish (made of silica or porcelain) of atleast 100ml capacity.

Ignite at 550+ or -50 C in a muffle furnace of half an hour for to remove any
moisture content present in the dish, cool in a dessicator and weigh initial weight
of the dish.

Take 50ml of unfiltered sample in the pre-weighed dish and evaporate it on a

water bath at 100-110C or a hot plate having temperature not more than 98
degree for completely drying the residue.

After completely drying the residue, placed it on a dessicator for cooling.

Take the final weight of dish after cooling in a dessicator.

The total solids concentration is equal to the difference between the weight of the
dish with the residue and the weight of the dish without it.

CALCULATION:

29
 Total Solids (mg/L) = (A B) 1000 1000

Where,

A = Final weight of the dish in grams

B = Initial weight of the dish in grams

V = Volume of the sample taken in ml

30
 TOTAL DISSOLVED SOLIDS

Total Dissolved Solids (TDS) are solids in water that can pass through a filter (usually
with pore size 0.45 micrometers). TDS is a measure of the amount of material dissolved in water.
This material can include carbonate, bicarbonate, chlorides, sulphates, phosphates, nitrates,
calcium, magnesium, sodium, organic ions and other ions. A certain level of these ions in water
is necessary for aquatic life. Changes in TDS concentrations can be harmful because the density
of water determines the flow of water into and out of organisms cells. However, if TDS
concentrations are too high or too low, the growth of much aquatic life can be limited and death
may occur.

31
 Similar to TSS, high concentrations of TDS may also reduce water clarity, contribute to a
decrease in photosynthesis, combine with toxic compounds and heavy metals and lead to an
increase in water temperature. TDS is used to estimate the quality of drinking water, because it
represents the amount of ions in the water. Water with high TDS has a bad taste and with high
levels of hardness could result in a laxative effect.
Dissolved solids refer to any minerals, salts, metals, cations or anions dissolved in water.
Total dissolved solids (TDS) comprise inorganic salts (primarily calcium, magnesium,
potassium, sodium, bicarbonates, chlorides and sulphates) and some small amounts of organic
matter that are dissolved in water.
TDS in drinking water originate from natural sources, sewage, urban runoff, industrial
wastewater, and chemicals used in the water treatment process, and the nature of the piping or
hardware used to convey the water, i.e. the plumbing. In the U.S. elevated TDS has been due to
natural environmental features such as mineral springs, carbonate deposits, salt deposits, and sea
water intrusion, but other sources may include salts used for road de-icing, drinking water
treatment chemicals, storm water and agricultural runoff, and point/non-point wastewater
discharges.

PRINCIPLE:

Total Dissolved Solids are determined as the residue left after evaporation of the filtered
sample.

APPARATUS:

1. Water bath

2. Dessicator

PROCEDURE:

Take an evaporating dish (made of silica or porcelain) of atleast 100ml capacity.

Ignite at 550+ or -50 C in a muffle furnace of half an hour for to remove any
moisture content present in the dish, cool in a dessicator and weigh initial weight
of the dish.

32
 Take 50ml of filtered sample in the pre-weighed dish and evaporate it on a water
bath at 100-110C or a hot plate having temperature not more than 98 degree for
completely drying the residue.

After completely drying the residue, placed it on a dessicator for cooling.

Take the final weight of dish after cooling in a dessicator.

The total dissolved solids concentration is equal to the difference between the
weight of the dish with the residue and the weight of the dish without it.

CALCULATION:

Total Dissolved Solids (mg/L) = (A B) 1000 1000

Where,

A = Final weight of the dish in grams

B = Initial weight of the dish in grams

V = Volume of the sample taken in ml

33
 TOTAL SUSPENDED SOLIDS

Total Suspended Solids (TSS) is solids in water that can be trapped by a filter. TSS can
include a wide variety of material, such as silt, decaying plant and animal matter, industrial
wastes, and sewage. High concentrations of suspended solids can cause many problems for
stream health and aquatic life.

High TSS can block light from reaching submerged vegetation. As the amount of light
passing through the water is reduced, photosynthesis slows down. Reduced rates of
photosynthesis causes less dissolved oxygen to be released into the water by plants. If light is
completely blocked from bottom dwelling plants, the plants will stop producing oxygen and will
die. As the plants are decomposed, bacteria will use up even more oxygen from the water. Low
dissolved oxygen can lead to fish kills. High TSS can also cause an increase in surface water
temperature, because the suspended particles absorb heat from sunlight. This can cause dissolved
oxygen levels to fall even further (because warmer waters can hold less DO), and can harm
aquatic life in many other ways.

High TSS in a water body can often mean higher concentrations of bacteria, nutrients,
pesticides, and metals in the water. High TSS can cause problems for industrial use, because the
solids may clog or scour pipes and machinery.

The flow rate of the water body is a primary factor in TSS concentrations. Fast running
water can carry more particles and larger-sized sediment. Heavy rains can pick up sand, silt, clay,
and organic particles (such as leaves, soil, and tire particles) from the land and carry it to surface
water. A change in flow rate can also affect TSS; if the speed or direction of the water current
increases, particulate matter from bottom sediments may be resuspended.

34
PRINCIPLE:
Total Suspended Solids (TSS) are solids in water that can be trapped by a filter.

PROCEDURE:
To measure Total Suspended Solids, the water sample is filtered through a pre-
weighed filter paper. The residue retained on the filter paper is dried in an oven at
103 to 105 C until the weight of the filter paper no longer changes. The increase
in weight of the filter paper represents the total suspended solids.

Total Suspended Solids (TSS) can also be measured by for total solids and
subtracting total dissolved solids.

TSS = TS TDS

SUSPENDED PARTICULATE MATTER IN AMBIENT AIR

Ambient concentrations of particulate matter of less than 10 m aerodynamic diameter

were measured in Switzerland for a 1 yr period in 1993 at a dozen urban, rural and alpine sites.
PM10 concentrations ranged between 10 g m3 (alpine) and 33 g m3 (urban). Highest
concentrations were found at Lugano, in the south of the Alps. Alpine sites showed considerably
lower levels. The ratios between PM10 and TSP were found to be between 0.6 and 0.75 and the
highest ratios were found in the most polluted urban sites. Seasonal variation of particulate
pollution showed peak levels during winter and autumn, mainly during cold temperature-
inversions. Statistical analyses have shown a good correlation between PM 10 and NO2 and SO2,
and TSP in urban areas.
PM2.5 and PM10 particles easily penetrate into the airways and lungs where they may
produce harmful health effects such as the worsening of heart and lung diseases. The risk of
these health effects is greatest in the elderly and the very young. Exposure to elevated
concentrations of PM is also associated with increased hospital and doctor visits and increased
numbers of premature deaths.
Several studies have demonstrated a relationship between levels of airborne particulate
matter less than 10 or 2.5 microns in aerodynamic diameter and acute asthma severity indices
including hospital admissions, decline in pulmonary function, and increased medication use and
symptoms. This study went further and looked at the effect of concurrent tobacco smoke
exposure on the potential adverse effects of particulate particle exposure.

PRINCIPLE:

35
 Air is drawn through a size-selective inlet and through a 20.3 X 25.4 cm (8 X 10 in) filter
at a flow rate, which is typically 1132 L/min. Particles with aerodynamic diameter less than the
cut-point of the inlet are collected by the filter. The mass of these particles is determined by the
difference in filter weights prior to and after sampling. The concentration of PM 10 in the
designated size range is calculated by dividing the weight gain of the filter by the volume of air
sampled.

REQUIREMENT:
The following items are necessary to perform the monitoring and analysis of Particulate
Matter PM10 in ambient air:
Analytical balance
Sampler : High Volume Sampler with size selective inlet for PM10 and
automatic volumetric flow control
Calibrated flow-measuring device to control the airflow at 1132 L/min.
Top loading orifice kit
Filter Media A Glass fibre filter of 20.3 X 25.4 cm (8 X 10 in) size
Dessicator

INSTRUMENTATION AND WORKING:

Tilt back the inlet and secure it according to manufacturer's instructions. Loosen the
faceplate wing nuts and remove the faceplate. Remove the filter from its jacket and centre it on
the support screen with the rough side of the filter facing upwards. Replace the faceplate and
tighten the wing nuts to secure the rubber gasket against the filter edge. Gently lower the inlet.
For automatically flow-controlled units, record the designated flow rate on the data sheet. Record
the reading of the elapsed time meter. The specified length of sampling is commonly 8 hours or
24 hours. During this period, several reading (hourly) of flow rate should be taken. After the
required time of sampling, record the flow meter reading, take out the filter media from the
sampler, and put in a container or envelope.

SAMPLE ANALYSIS:
Filter inspection: Inspect the filter for pin holes using a light table. Loose particles should
be removed with a soft brush. Apply the filter identification number or a code to the filter if it is
not a numbered. Condition the filter in conditioning room maintained within 20-30 C and 40-
50% relative humidity or in an airtight dessicator for 24 hours. Take initial weight of the filter
paper (Wi) before sampling. Condition the filter after sampling in conditioning room maintained
within 20-30 C and 40-50% relative humidity or in an airtight dessicator for 24 hours. Take final
weight of the filter paper (Wf).

CALIBRATION:
Periodical calibration of the sampler is being done by Orifice Transfer Standard - The
PM10 sampler calibration orifice consists of a 3.175 cm (1.25 in) diameter hole in the end cap of

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7.62 cm (3 in) diameter by 20.3 cm (8 in) long hollow metal cylinder. This orifice is mounted
tightly to the filter support in place of the inlet during calibration. A small tap on the side of the
cylinder is provided to measure the pressure drop across the orifice. A flow rate of 1132 L/min
through the orifice typically results in a pressure difference of several inches of water. The
relationship between pressure difference and flow rate is established via a calibration curve
derived from measurements against a primary standard such as a Roots meter at standard
temperature and pressure. Flow resistances that simulate filter resistances are introduced at the
end of the calibrator opposite the orifice by a set of perforated circular disks.

FLOW CHART FOR MEASUREMENT OF PM10:

Check the filter for any physical damages

Mark identification number on the filter

Condition the filter in conditioning room / dessicator for 24 hours

Record initial weight

Place the filter on the sampler

Run the sampler for eight hours

Record the flow rate on hourly basis

Remove the filter from the sampler

Keep the exposed filter in a proper container

Record the total time of sampling & average flow rate

Again condition the filter in conditioning room / desiccators for 24 hours

Record final weight

Calculate the concentration of PM10 in g/m3

CALCULATION:

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 CPM10 g/m3 = (Wf Wi) x 106 / V

Where,
C PM10 = Concentration of Nitrogen dioxide, g/m3
Wf = Initial weight of filter in g
Wi = Initial weight of filter in g
106 = Conversion of g to g
V = Volume of air sampled, m3

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