ABSTRACT

Water is perhaps the most precious natural resource after air. Though the surface of the
earth is mostly consists of water, only a small part of it is usable, which makes this
resource limited. This precious and limited resource, therefore, must be used with car e.
As water is required for different purposes, the suitability of it must be checked before
use. Also, sources of water must be monitored regularly to determine whether they are in
sound health or not. Poor condition of water bodies are not only the indictor of
environmental degradation, it is also a threat to the ecosystem. In industries, improper
quality of water may cause hazards and severe economic loss. Thus, the quality of water
is very important in both environmental and economic aspects. Thus, water quality
analysis is essential for using it in any purpose. After years of research, water quality
analysis is now consists of some standard protocols. There are guidelines for
sampling, preservation and analysis of the samples. Here the standard chain of action is
discussed briefly so that it may be useful to the analysts and researchers.
In this work, samples of water were collected from three different tube-wells at two
different times of the year. The first set of samples was collected in the month of
September, 2019 & the second set was collected in April, 2020. Over the due course of
time various parameters regarding the water quality were analysed & the Indian
Standards: 10500 (Drinking water specifications) was referred to in order to check the
acceptability of water.
The parameters which were analysed are as follows :
 Total Dissolved Solids

 Total Suspended Solids

 Determination of pH

 Determination of chloride content

 Conductivity

 Determination of sulphate content

 Turbidity

 Iron content

 Manganese content

1
Most of the parameters were not found to be in the desirable range for drinking water &
hence, appropriate measures were suggested to improve the quality of water.

The purpose of this Project is to find out, how the water sample can test. The report starts
with introduction and ends with conclusion with experiment report. The report defines the
detailed information about water testing with various examples. The report also explains
about the quantity of the samples and types of the samples. The Sampling Methods
consists of Manual sampling, Automatic sampling and Sorbent sampling, which explain
the details of water testing.
The physical and chemical properties of drinking water vary from top to bottom of the
depth of the earth, and the time from morning to night. It is therefore difficult to obtain a
truly representative sample. We need water for different purposes; we need water for
drinking, industry, irrigation, swimming, fishing, etc. Water for various purposes
requirements for the composition and purity, and each body of water must be tested
regularly to confirm the suitability.
The types of analysis could change from simple field testing for a single analytic to
laboratory based multi component instrumental analysis. The analytical process demands
sampling and sample storage since changes in composition of water do not stop once the
sampling has been taken. Screening is done to ensure that water reaches the laboratory,
the same composition as it has occurred during sampling.

2
Introduction

Ideally, a laboratory infrastructure should be established which will enable all samples to
be returned to a central or regional laboratory within a few hours of being taken.
However, this depends on the availability of a good road system and of reliable motorized
transport for all sampling officers, and these are not available in many countries. Thus,
although it may be possible to establish well-equipped central and even regional
laboratories for water analysis, at the provincial and district levels it may be necessary to
rely on a relatively small number of simple tests. As noted in Chapter 1, this approach is
sometimes called critical-parameter
water testing. The most important factor to take into account is that, in most communities,
the principal risk to human health derives from faecal contamination. In some countries
there may also be hazards associated with specific chemical contaminants such as fluoride
or arsenic, but the levels of these substances are unlikely to
change significantly with time. Thus, if a full range of chemical analyses is undertaken on
new water sources and repeated thereafter at fairly long intervals, chemical contaminants
are unlikely to present an unrecognized hazard. In contrast, the potential for faecal
contamination in untreated or inadequately treated community supplies is always present.
The minimum level of analysis should therefore include testing for indicators of faecal
pollution (thermotolerant (faecal) coliforms), turbidity, and chlorine residual and pH (if
the water is disinfected with chlorine).
Even in developing countries poorly served by roads and transportation, it is usually
possible to devise a rational sampling and analytical strategy. This should incorporate
carefully selected critical-parameter tests in remote (usually rural) locations using simple
methods and portable water-testing equipment (see pp. 65–66) where appropriate.
Wherever possible the community should be involved in the sampling process. Where
water is disinfected, primary health workers, schoolteachers, and sometimes community
members can be trained to carry out simple chlorine residual testing. The same people
could also collect samples for physicochemical analysis and arrange for their delivery to
the regional laboratory.
The use of community members in this way has significant implications for training and
supervision but would be one way of ensuring more complete surveillance coverage.

3
Water quality
Water quality refers to the chemical, physical and biological characteristics of water. It is
a measure of the condition of water relative to the requirements of one or more biotic
species and or to any human need or purpose. It is most frequently used by reference to a
set of standards against which compliance can be assessed. The most common standards
used to assess water quality relate to health of ecosystems, safety of human contact and
drinking water.
Different properties were analysed & compared during the course of the project.
Some of the properties analysed are as follows –
 Total Dissolved Solids

 Total Suspended Solids

 Determination of pH

 Determination of chloride content

 Conductivity

 Determination of sulphate content

 Turbidity

 Iron content

 Manganese content

Sampling:
The physical and chemical characteristics of drinking water vary from top to bottom of
depth of land, as well as with time as from morning to evening. It therefore becomes
difficult to obtain a truly representative sample.

Types of samples:
a) Grab sample: Grab samples are single samples collected at a specific spot at a site over
a short period of time (typically seconds or minutes).

b) Composite samples: Composite samples should provide a more representative

sampling of heterogeneous matrices in which the concentration of the analysis of interest
may vary over short periods of time and/ or space. Composite samples can be obtained by
4
combining portions of multiple grab samples or by using specially designed automatic
sampling devices.

Sampling Methods:
a) Manual sampling: Manual sampling involves minimal equipment but may be costly
and time-consuming for routine or large-scale sampling programs.
b) Automatic sampling: Automatic samplers can eliminate can reduce labor costs, may
provide the means for frequent sampling and are used increasingly.

c) Sorbent sampling: Use of solids sorbent s, particularly membrane type disks, is

becoming more frequent. These methods offer advantages of rabid, inexpensive sampling
if the analytes of interest can be adsorbed and desorbed efficiently and the water matrix is
free of particulates that plug the sorbent

Source of sample:
Sample collected from bore water inVALLAM 27.11.10 and testing conducted on
02.11.10.
Sample containers:
Containers typically are made of plastic or glass, but one material may be preferred over
the others. For example, silica, sodium, and boran may be leached from soft glass but not
plastic, and trace levels of some pesticides and metals may absorb onto the walls of glass
containers. Thus hard glass container is preferred. For samples, containing organic
compounds, do not use plastic containers expect those made of fluorinated polymers such
as polytetrafluoroethylene (PTFE).

Sample Volumes:
Collect a 1 litre sample for most physical and chemical analyses. Do not use sample from
the same container for multiple testing requirements (e.g., organic, inorganic,
radiological, bacteriological, and microscopic examinations) because methods of
collecting and handling are different for each type of test.
Always collect enough sample volume in the appropriate container in order to compile
with the sample handling, storage and preservation requirements.

5
Time interval between collection and analysis:
In general, the shorter the time that elapses between collection of a sample and its
analysis, the more reliable will be analytical results. For certain constituents and physical
values, immediate analysis in the field is required. For composited sample it is common
practice to use the time at the end of composite collection as the sample collection time.

Preservation Techniques:
To minimize the potential for volatilization or biodegradation between sampling and
analysis, keep samples as cool as possible without freezing. Preferably pack samples in
crushed or cubed ice or commercial ice substituent before shipment. Avoid using dry to
break. Dry ice also may effect a pH change in samples. Keep composite samples cool
with ice or a refrigeration system set at 4˚C during compositing. Analyze samples as
quickly as possible on arrival at the laboratory. If immediate analysis is not possible,
preferably store at 4˚C.

DETERMINATION OF pH
AIM:
To determine the pH of a given sample of water.
APPARATUS REQUIRED:
1) Ph meter with electrode

2) Beakers

3) 100 ml standard flasks

4) Funnels

5) Tissue papers

6) Wash bottle

CHEMICALS REQUIRED:
1) Distilled water

2) Buffer tablets pH values of 4.0

3) Buffer tablets pH values of 7.0

6
4) Buffer tablets pH values of 9.2

REAGENT PREPARATIONS:
Standard Buffer Solutions:
They can be prepared easily by dissolving the pH powder or tablets completely in 100ml
of distilled water.

PRINCIPLE:
pH unit of measure which describes the degree of acidity or alkalinity of a solution. It is
measured on a scale of 0to 14. The term pH is derived from P the mathematical symbol of
the negative logarithm, and H the chemical symbol of the Hydrogen. The formal
definition of pH is the negative logarithm of the hydrogen ion activity.
pH= -log10[H+]
pH provides the needed quantitative information by expressing the degree of the activity
of an acid or base in terms of hydrogen ion activity.

THEORY:
Fresh distilled water has a pH of 7. Acidic waters have a pH of 0to 7, whereas alkaline
waters have a pH of 7 to 14. Ammonia and Lime solution have pH of about 12 where as
many cool drinks, lime juice, battery, etc. have pH of less than 4. As pH is measured on a
logarithmic scale, a water having a pH of 6to 10 times more acidic than the natural water,
a water having a pH of 4 is 1000 times more acidic than water with pH 7 and a pH of 2 is
100000 times more acidic than a pH of 7.
pH of a solution can be found easily by using pH strips (paper) or a pH meter gives very
accurate values whereas pH strips gives approximate values. pH is determined by the
measurement of electromotive force of a cell comprising an indicator electrode
responsive to hydrogen ions (such as glass electrode) immersed in the test solution and a
reference electrode is usually achieved by means of a liquid junction, which forms a part
of the reference electrode. The ‘emf’ of this cell is immersed with pH meter. This is high
impedance electrometer calibrated in terms of pH.

7
SPECIFICATION:
Range : 0-14pH
Accuracy : 0.01 pH (1digit)
Resolution : 0.01 pH
Temp.Compensation :0to100 Degree C. (Manual).

PROCEDURE:
Connect the pH electrode to the input socket at the front. Clean the electrode with
distilled water and dry it. Dip the electrode in the 4.00 pH buffer solution which is
provided. Measure the temperature of the buffer solution. Keep the TEMP. Knob at
temperature of the solution. Push the pH switch. Adjust the display to 4.00 pH with the
CAL knob. Now the instrument is calibrated. Wash the electrode, dry it and put it in the
solution whose pH is to be measured.

RESULT:
pH of the given samples=7.27

SIGNIFICANCE:
1) Knowing pH value is very important parameter for analysis of water/waste water and
its suitability for domestic use and for irrigation. Certain chemical and biological
processes work only at a particular pH. of 6.5 to 8.5 has no direct adverse effect on
health. However a lower value below will produce
sour taste and higher value above 8.5 a bitter taste. Higher value of pH encourages the
potential of chlorine. High pH induces the formation of trihalomethanes which are
causing cancer in human beings. According to BIS water for domestic consumption
should have a pH between 6.5 to 8.5.

2) Corrosion of water mains is the main problem associated with acidic waters.

3) Acidic/alkaline waters cannot be used for contraction purpose also. If pH is less algae
die, fish cannot reproduce and it causes acidity, corrosion, and irritation of mucous
membranes, tuberculosis and further health problems in humans.

8
Location of sampling points
One objective of surveillance is to assess the quality of the water supplied by the supply
agency and of that at the point of use, so that samples of both should be taken. Any
significant difference between the two has important implications for remedial strategies.
Samples must be taken from locations that are representative of the water source,
treatment plant, storage facilities, distribution network, points at which water is delivered
to the consumer, and points of use. In selecting sampling points, each locality should be
considered individually; however, the following general criteria are usually applicable:
• Sampling points should be selected such that the samples taken are representative of the
different sources from which water is obtained by the public or enters the system.
• These points should include those that yield samples representative of the conditions at
the most unfavourable sources or places in the supply system, particularly points of
possible contamination such as unprotected sources, loops, reservoirs, low-pressure
zones, ends of the system, etc.
• Sampling points should be uniformly distributed throughout a piped distribution system,
taking population distribution into account; the number of sampling points should be
proportional to the number of links or branches.
• The points chosen should generally yield samples that are representative of the system
as a whole and of its main components.
• Sampling points should be located in such a way that water can be sampled from reserve
tanks and reservoirs, etc.
• In systems with more than one water source, the locations of the sampling points should
take account of the number of inhabitants served by each source.
• There should be at least one sampling point directly after the clean-water outlet from
each treatment plant.
Sampling sites in a piped distribution network may be classified as:

 fixed and agreed with the supply agency;

 fixed, but not agreed with the supply agency; or
 random or variable.
Each type of sampling site has certain advantages and disadvantages. Fixed sites agreed
with the supplier are essential when legal action is to be used as a means of ensuring
improvement; otherwise, the supply agency may object to a sample result on the grounds

9
that water quality may have deteriorated in the household, beyond the area of
responsibility of the supplier. Nevertheless, fixed sample points are rare or unknown in
some countries.
Fixed sites that are not necessarily recognized by the supply agency are used frequently in
investigations, including surveillance. They are especially useful when results have to be
compared over time, but they limit the possibility of identifying local problems such as
cross-connections and contamination from leaking istribution networks.
Sampling regimes using variable or random sites have the advantage of being more likely
to detect local problems but are less useful for analysing changes over time.

Sampling frequency
The most important tests used in water-quality surveillance or quality control in small
communities are those for microbiological quality (by the measurement of indicator
bacteria) and turbidity, and for free chlorine residual and pH where chlorination is used.

AIM:
To determine the amount of turbidity present in the sample of water by using Nephelo
Turbidity meter.
APPARATUS REQUIRED:
1) Nephelometric turbidity meter,

2) Nessler’s tubes with stand,

3) Standard flasks,

4) Wash bottle.

CHEMICALS REQUIRED:
1) Distilled Water

2) Hydrazine sulphate,

3) Hexamethylenetetramine

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PREPARATION OF STOCK STANDARDS:
The particles of formation are uniform in size and shape. The stock standards prepared
from the formations are accurate within 1% and stable for 6-8 weeks. The stock standard
of 4000NTU is prepared as per the following procedure.
1) Take 5g of reagent grade Hydrazine Sulphate and dissolve in 400 of distilled water.
This is solution A.

2) Next dissolve 50g of pure HexamethyleneTetramine in 400 ml of distilled water. This

is solution B.

3) Mix solution A and B and make it upto one litre by adding distilled water and allow
this mixture to settle for 48 hours at normal room temperature.
This is a stock standard of 4000 NTU and can be used for 6-8 months to prepare working
standards as per following table. Shake this solution well before making dilution.

PRINCIPLE:
The tungsten filament produces a converging light beam. It is then scattered by the
suspended particles present in the given sample of water. The scattered light is sensed by
a photo cell kept at 90 in light path and the amount of scattered light is a direct measure
of tubidity of the solution.
As table and regulated DC supply is used to excite the lamp. Similarly a high gain
amplifier is used to convert the photocell output into measurable signal.

11
THEORY:
Turbidity is a measure of the transparency of the water. Turbidity is the property of water
because of which it offers resistance to passage of light. It is caused by suspended solids
(such as silt and clay), living or dead algae and other microorganisms. It depends on the
type of soil over which water has run and the velocity of run-off. As sand is a good
filtering methods, ground waters are less turbid. River/ canal waters are highly turbid
(upto 300 NTU) during monsoon. River water have negligible turbidity during summer,
as river flow is mostly contributed by ground water during summer. Turbidity is
measured by “Turbidity Rod” or “Jackson Turbidity Meter” (in JT Units) or by
“Nephelometer” (in NT Units ). Insoluble particles of soil, organics, micro-organisms and
other inorganic material, impede the passage of light by scattering and absorbing rays.
The scattering of light is generally proportional to the turbidity. The turbidity is thus
measured from the amount of light scattered by the sample taking a reference with
standard turbidity suspension. Turbidity is expressed as the amount of suspended matter
in liquid in parts per million or milligrams per liter, determine by the optical observations.
The standard unit of turbidity is “that produced by one part of finely dissolved silica in
one million parts of distilled water” for potable water allowable turbidity is between 5 to
10 mg/l.

SPECIFICATION:
Range: From 0to 500 NTU in four
decade range of , 10, 1CO and 500 NTU

Accuracy :+ 1% of full scale in 10 & 100 NTU range

+ 2% of full scale in 1 & 500 NTU ranges.
Drift/ Oscillation :0.02 NTU due to particle movement
Supply:230V AC + 10% at 50 Hz
Power Consumption :25VA approx.

PROCEDURE:
Three pin plug of the instrument was introduced into the appropriate main socket. The
instrument was switched on and it was allowed to warm up for 10 to 15 minutes. The
appropriate range is selected and standardize control was kept maximum. The test tube
with distilled water was inserted into the cell holder and it is covered with light shield.
12
Now set zero control was adjusted to indicate zero in the meter. The test tube containing
distilled water is removed and was replaced with the test tube containing standard
solution. The standard axliseel controller was adjusted, such that the meter indicate 100 in
accordance with the appropriate range in standard solution. The test tube containing the
sample solution was inserted into the cell holder and the corresponding reading was noted
in NTU units.

RESULT:
The turbidity in sample water=5.3NTU

PRECAUTIONS:
1) The instrument should be kept and operated in environment free from corrosive acid
fumes and excessive moisture for prolonged life.

2) Ensure that instrument GROUND pin is connected to real ground through supply
socket.

3) Test tubes are cleared with detergent and rinsed with distilled water prior to wiping off
with tissue paper. The cleaning of the test tubes is very essential while standardizing
instrument for 0-1 NTU range.

4) Align the marking of test tube and cell holder for accurate readings.

5) Use high grade distilled water to get accurate results. The performance of instrument in
0-1 NTU range is greatly independent on the quality of distilled water. It is preferable to
use triple distilled water.

6) Keep the tube holder covered with light shield when not in use.

13
DETERMINATION HARDNESS
AIM:
To determine the total hardness of the given sample of water.
APPARATUS REQUIRED:
1. Burette,

2. Pipette,

3. Conical flask,

4. Beakers,

5. Standardflask,

6. PVC bottle.

CHEMICALS REQUIRED:
1.EDTA,
2. Ammonium chloride,
3. Ammonium hydroxide ,
4. EBT,
5. Sodium chloride,
6. Ethanol.

REAGENT PREPARATIONS:
1. EDTA solution 0.01N:
Dissolve 3.723g of disodium salt of EDTA in distilled water to prepare 1liter of solution.
Store in polyethylene or Pyrex bottle.
2. Buffer solution:
Dissolve 16.9g of ammonium chloride in 143ml of concentrated ammonium hydroxide.
Add 1.25g of magnesium salt of EDTA to obtain sharp change in color of indicator and
dilute to 1 liter with distilled water.
3. Erichrome Black T:
Dissolve 0.25g of EBT in 500ml alcohol or 0.5g of EBT with 100g sodium chloride (A.R)
to prepare dry powder.

14
PRINCIPLE:
Hardness is generally caused by the calcium and magnesium ions present in water.
Polyvalent ions of some other metals like strontium, iron, aluminum, 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 which are far
higher in qualities over other hardness producing ions.
Calcium, and magnesium form a complex of wine red color with Erichrome black t at ph
of 10.0+0.1 the EDTA has g0t a stronger affinity towards ca++ and mg++ and, therefore
by addition of EDTA, the former complex ion broken down and a new complex of blue
color is formed.

PROCEDURE:
TITRATION:
EDTA VsSAMPLE WATER
To pipette out 20ml of sample water into a clean conical flask. To this 5ml of buffer
solution and 2drops of Erichrome Black T indicator was added. The solutionwas titrated
against EDTAtaken in the burette. The end point was change of color from wine red to
steel blue.Thetitration was repeated upto concordant values.

RESULT:
The hardness of given sample of water 577.5 mg/l

15
SIGNIFICANCE:
1. Absolutely soft water are tasteless (e.g. Distilled water). On the other hand, hardness
up to 600 mg/l can be relished if got acclimatized to.
2. Moderately hard water is prepared to soft water for drinking and irrigation purposes.

3. Hard water from scales in hot water pipes and boilers. They are difficult to be removed
and lot of heat energy is wasted if these scales are not removed.

4. Soft water affects the human cardiovascular system and causes heart- attacks.

5. Soft water has a flat taste. Soft water tends to become acidic and has corrosive action.
It dissolves toxic elements such as lead easily.

6. The precipitate formed by soap and hard water adheres to surface of tubes, sinks and
utensils and stain clothes and dishes.

DETERMINATION OF RESIDUAL CHLORINE

AIM:
To determine the residual chlorine present in the given sample of water.
APPARATUS:
1. Conical flasks,

2. burette, pipette,

3. Standard flask.

CHEMICALS REQUIRED:
a. Acetic acid,

b. Potassium Iodide,

c. Sodium thiosulphate,

d. Starch.

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REAGENT PREPARATIONS:
1. Sodium thiosulpahte solution 0.025N:

Dissolve 1.575 g of sodium thiosulphate in distilled water and make upto 1 liter.
2. Starch Indicator:

Dissolve 2 g of L.r grade soluble starch in distilled water and pour this emulsion into 100
ml of boiling water. Allow to boil for few minutes, add 0.2 g of salicylic acid as
preservative. Cool this solution and then use.

PRINCIPLE:
Chlorine is primarily added to the water for destroying the harmful micro organisms,
presence of excess chlorine intensities the taste and odours of many other compound such
as phenol, etc., It may also be harmful to many aquatic microorganisms in combination
with ammonia.
Chlorine is a strong oxidizing agent and liberates iodine from potassium iodide. The
liberated iodine is equivalent t the amount of chlorine and can be titrated against sodium
thiosulphate using starch as an indicator.
PROCEDURE:
Take 100 ml sample of water in a conical flask and add 5ml acetic acid. The pH after
addition of acetic acid should be between 3 and 4.
Add approximately 1 g of KI crystals and mix thoroughly with a stirring rod for about 15
minutes keeping it away from the direct sunlight. Add a few drops of starch indicator and
titrates against 0.025N sodium thiosulphate until the contents turns colorless from blue.

17
RESULT:
Amount of residual chlorine present in the given sample is =17.75mg/l
REFERENCE:
IS 3025 ( part 26 ) – 1986 methods of sampling and test (physical and chemical) for water
and waste water- Residual Chlorine.

DETERMINATION OF CHLORIDES
AIM:
To determine the concentration of chlorides present in the given sample of water.
APPARATUS REQUIRED:
o Conical flasks,

o Burette

o Pipette,

o Standard flask,

o Funnel

18
o Wash bottle.

CHEMICALS REQUIRED:
a. Silver nitrate

b. Potassium chromate

c. Sodium chloride

REAGENT PREPARARTIONS:
1) Silver Nitrate 0.02N:

1) Dissolve 3.4 g of dried silver nitrate in distilled water to make 1liter of the solution and
keep in a dark bottle.
2) Potassium chromate 5%:
Dissolve 5 g of potassium chromate in 100 ml distilled water.
3) Sodium chloride 0.0141N:

Dissolve 4.121 g of anhydrous Sodium chloride in 250 ml distilled water.

PRINCIPLE:
Silver nitrate reacts with chloride to form very slightly soluble white precipitate of AgCl2
. At the and point when all the chloride get precipitated, free silver ions react with
chromate to form silver chromate of reddish brown color.

PROCEDURE:
TITRARTON:
SAMPLE WATER Vs SILVER NITRATE
20 ml of sample water pipette out into a clean conical flask. One drop of potassium
dichromate was added as a indicator. The solution turns yellow in color. The solution was
titrated against silver nitrate taken in the burette. The end point was the change of yellow
color into reddish brown color. Titration was repeated upto its concordant values.

19
Amount of chloride present in the given sample of water=0.033 N
Normality of sample water X Equivalent weight of silver nitrate X 1000
=0.00537X39.5X1000
=212.043 mg/l

RESULT:
The amount of chloride present in the given sample of water=212.043 mg/l
REFERENCE:
IS 3025 (part 32)-1988 Methods of sampling and test (physical and chemical) for water
and waste water- Chloride.

DETERMINATION OF SULPHATE
AIM:
To estimate the concentration if sulphate in the given sample of water.

20
APPARATUS REQUIRED:
1) Silica crucible,

2) Desiccators,

3) Ash less filter paper,

4) Beaker.

CHEMICALS REQUIRED:
1) Methyl red,

2) Hydrochloric acid,

3) Silver Nitrate,

4) Nitric acid.

REAGENT PREPARATIONS:
1.Methyl red indicator:
Dissolve 100 mg of methyl red sodium salt in distilled water to prepare 100 ml of
solution.
2.Hydrochloric acid:
HCl (1:1)
3. Barium chloride solution:

Dissolve 100 g BaCl2.H2O in distilled water to prepare 1 liter of solution. Filter the
solution through a filter paper before use.
4.Silver nitrate-nitric acid reagent:
Dissolve 8.5 g of AgNO3 and 0.5 ml concentrated HNO3 in distilled water to prepare 500
ml reagent.

PRINCIPLE:
Sulphate is precipitated as barium sulphate in the hydrochloric acid medium by addition
of barium chloride solution. The reaction is carried out near the boiling temperature. The
precipitation is filtered, washed to remove the chlorides, cried or ignited and weighed as
BaSO4.

21
Many substances interfere in performing this test. Suspended matter, Silica, nitrate and
sulphate lead to the positive errors where the results are on the higher side. Alkali metal
sulphate causes the low results. Presence of other metals such as iron and chromium also
yield low results due to the formation of metals sulphates.

PROCEDURE:
1) If the sample consist more than 25 ml/l of silica, it is to be removed prior to the
analysis for sulphate.

2) For removal of silica, evaporator the suitable volume of sample to dryness in platinum
dish on a water bath. Rotating the dish. Dry to contents again by evaporation and for final
drying deep the dish at 180 degree Celsius in an oven. If some organic matter is also
present, it can be burden over a flame at this stage. Now add 2 ml of dryness on a water
bath. Add 2 ml of HCl and
transfer it in hot water and filter. Wash the filter paper having silica. Several times with
hot distilled water and collect the combined filtrate.

3) Adjust the volume of the filtrate so that 50 mg sulphate should be in 250 ml volume. If
silica is present is less than 25 mg/l, there is no need of removal of it and suitable volume
of sample (100-150 ml0 can directly be taken for estimation of sulphates.

4) Add a few drop of methyl red to the sample and adjust the pH to 4.5-5.0 by addition of
HCl until the color changes to the orange. Add additional 1-2 ml of HCl.

5) Boil the solution and add warm BaCl2 solution in excess until the precipitation is
completes.

6) Heat the precipitation at 80-90 degree Celsius for at least 2 hours or more.

7) Filter the precipitation through the ash less filter paper by adding some pulp of the
same filter paper as a aid for filtration.

8) Wash the precipitate repeatedly with warm distilled water until the filtrate is free from
chloride which can be tested by AgNO3 solution. In the presence of chloride AgNO3
gives a white turbidity.

9) Dry the filter paper containing precipitate and ignite it in a crucible at 800 degree
centigrade for about 1 hour. Cool it in a desiccators and weight the precipitate of BaSO4.

22
RESULT:
Sulphate content of the given sample is = 0.41 mg/l

REFERENCE:
IS 3025 (part 24 )- 1986 methods of sampling and test (physical and chemical for water
and waste water- sulphate.

7) DETERMINATION OF DISSOLVED OXYGEN

AIM: To determine the dissolved oxygen concentration in the given sample.
APPARATUS REQUIRED:
a. Dissolved Oxygen bottle with stopper

b. Burette

c. Pipette

REAGENT PREPARATIONS:
1.Sodium thiosulpahte solution 0.025N:
Dissolve 24.82 g of Na2S2O3 in boiled distilled water and make up the volume to 1 lit.
Add 0.4 g of borax or a pallet of NaOH as stabilizer. This is 0.1 N stock solution. Dilute I
to 4 times with boiled distilled water to prepare 0.025 N solution (250≥ 1000 ml). Keep in
a brown glass stopper bottle.

23
2. Alkaline potassium iodide solution:

Dissolve 100 g of KOH and 50 g of KI 200 ml of boiled distilled water.

3. Manganesesulphate solution:
Dissolve 100 g of MnSO4.4H2O in 200 ml of boiled distilled water and filter.
4. Starch solution:
Dissolve 1 g of starch in 100 ml of warm (80 C- 90 C) distilled water
And add a few drops of formaldehyde solution.
5. Sulphuric acid:
H2SO4 conc. (sp.gr.1.84)

PRINCIPLE:
The manganese sulphate reacts with the alkali (KOH or NaOH) to form a white
precipitate of manganese hydroxide which in the presence of oxygen, gets oxidized to a
brown color compound. In the strong acid medium magnetic ions are reduced by iodide
which 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.

PROCEDURE:
Water sample was filled in a dissolved oxygen bottle and 1 ml of manganese sulphate was
added with a help of pipette. To it 1 ml of alkaline potassium iodide solution was added.
If oxygen is present it will form brown. If oxygen was not present while precipitate of
manganese oxide was formed. The bottle was shake for 50-100 times.
Then the precipitation was allowed to settle down. 2 ml of conc.H2SO4 was shake
slowly. Till all the precipitate are dissolved leaving the solution transparent but yellow in
color. The contents are transformed to titration flask and was titrated against N/40 sodium
thiosulphate solution till light yellow color was obtained.
Then 2-3 drops of solution blue. Again sodium thiosulphate solution was added till the
solution become colorless note the volume of sodium thiosulphate used.

24
RESULT:
The dissolved oxygen concentration in the given sample of water is =3.02 mg/l
IS 3025 (part 38)-1989 Methods of sampling and test (physical and chemical ) for water
and waste water – Dissolved Oxygen.

25
26
27
28
Sampling methods for physicochemical analysis
Results of physicochemical analysis are of no value if the samples tested are not properly
collected and stored. This has important consequences for sampling regimes, sampling
procedures, and methods of sample preservation and storage. In general, the time between
sampling and analysis should be kept to a minimum. Storage in glass or polyethylene
bottles at a low temperature (e.g. 4 C) in the dark is recommended. Sample bottles must
be clean but need not be sterile. Special preservatives may be required for some analytes.
Residual chlorine, pH, and turbidity should be tested immediately after sampling as they
will change during storage and transport.

Bacteriological analysis
The principal risk associated with water in small-community supplies is that of infectious
disease related to faecal contamination. Hence, as described in Chapter 1, the
microbiological examination of drinking-water emphasizes assessment of the hygienic
quality of the supply. This requires the isolation and enumeration of organisms that
indicate the presence of faecal contamination. In certain circumstances, the same
indicator organisms may also be used to assess the efficiency of drinking-water treatment
plants, which is an important element of quality control. Other microbiological indicators,
not necessarily associated with faecal pollution, may also be used for this purpose.
The isolation of specific pathogens in water should be undertaken only by reference
laboratories for purposes of investigating and controlling outbreaks of disease. Routine
isolation in other circumstances is not practical. Detailed methods for use in
bacteriological analysis are described in Annex 5 (multiple-tube method), Annex 6
(membrane-filtration method), Annex 7 (onsite testing method), and Annex 8 (presence–
absence test).

29
Indicator organisms
The properties and significance of the commonly used faecal indicator bacteria are
described in detail in Volume 1; a summary is provided here. Escherichia coli is a
member of the family Enterobacteriaceae, and is characterized by possession of the
enzymes -galactosidase and -glucuronidase. It grows at 44–45C on complex
media, ferments lactose and mannitol with the production of acid and gas, and produces
indole from tryptophan. However, some strains can grow at 37 C but not at 44–45C,
and some do not produce gas. E. coli does not produce oxidase or hydrolyse urea.
Complete identification of the organism is too complicated for routine use, but a number
of tests have been developed for rapid and reliable identification. Some of these methods
have been standardized at international and national levels and accepted for routine use;
others are still being developed or evaluated.
Escherichia coli is abundant in human and animal faeces; in fresh faeces it may attain
concentrations of 109 per gram. It is found in sewage, treated effluents, and all natural

30
waters and soils subject to recent faecal contamination, whether from humans, wild
animals, or agricultural activity. Recently, it has been suggested that E. coli may be
present or even multiply in tropical waters not subject to human faecal pollution.
However, even in the remotest regions, faecal contamination by wild animals, including
birds, can never be excluded. Because animals can transmit pathogens that are infective in
humans, the presence of E. coli or thermotolerant coliform bacteria must not be ignored,
because the presumption remains that the water has been faecally contaminated and that
treatment has been ineffective.

Thermotolerant coliform bacteria

Thermotolerant coliform bacteria are the coliform organisms that are able to ferment
lactose at 44–45C; the group includes the genus Escherichia and some species of
Klebsiella, Enterobacter, and Citrobacter. Thermotolerant coliforms other than E. coli
may also originate from organically enriched water such as
industrial effluents or from decaying plant materials and soils. For this reason, the term
“faecal” coliforms, although frequently employed, is not correct, and its use should be
discontinued. Regrowth of thermotolerant coliform organisms in the distribution system
is unlikely unless sufficient bacterial nutrients are present, unsuitable materials are in
contact with the treated water, the water temperature is above 13 C, and there is no free
residual chlorine.
In most circumstances, concentrations of thermotolerant coliforms are directly related to
that of E. coli. Their use in assessing water quality is therefore considered acceptable for
routine purposes, but the limitations with regard to specificity should always be borne in
mind when the data are interpreted. If high
counts of thermotolerant coliforms are found in the absence of detectable sanitary
hazards, additional confirmatory tests specific for E. coli should be carried out.
National reference laboratories developing national standard methods are advised to
examine the specificity of the thermotolerant coliform test for E. coli under local
conditions.
Because thermotolerant coliform organisms are readily detected, they have an important
secondary role as indicators of the efficiency of water-treatment processes in removing
faecal bacteria. They may therefore be used in assessing the degree of treatment necessary
for waters of different quality and for defining
performance targets for removal of bacteria.
31
Coliform organisms (total coliforms)
Coliform organisms have long been recognized as a suitable microbial indicator of
drinking-water quality, largely because they are easy to detect and enumerate in water.
The term “coliform organisms” refers to Gram-negative, rod-shaped bacteria capable of
growth in the presence of bile salts or other surface-active
agents with similar growth-inhibiting properties and able to ferment lactose at 35–37C
with the production of acid, gas, and aldehyde within 24–48 hours.
They are also oxidase-negative and non-spore-forming and display -galactosidase
activity. Traditionally, coliform bacteria were regarded as belonging to the genera
Escherichia, Citrobacter, Enterobacter, and Klebsiella. However, as defined by modern
taxonomical methods, the group is heterogeneous. It includes lactosefermenting bacteria,
such as Enterobacter cloacae and Citrobacter freundii, which can be found in both faeces
and the environment (nutrient-rich waters, soil, decaying plant material) as well as in
drinking-water containing relatively high concentrations of nutrients, as well as species
that are rarely, if ever, found in faeces and may multiply in relatively good-quality
drinking-water, e.g. Serratia fonticola, Rabnella aquatilis, and Buttiauxella agrestis. The
existence both of non-faecal bacteria that fit the definitions of coliform bacteria and of
lactose-negative coliform bacteria limits the applicability of this group as an indicator of
faecal pollution. Coliform bacteria should not be detectable in treated water supplies and,
if found, suggest inadequate treatment, posttreatment contamination, or excessive
nutrients. The coliform test can therefore be used as an indicator both of treatment
efficiency and of the integrity of the distribution system. Although coliform organisms
may not always be directly related to the presence of faecal contamination or pathogens in
drinking-water, the coliform test is still useful for monitoring the microbial quality of
treated piped water supplies. If there is any doubt, especially when coliform organisms
are found in the absence of thermotolerant coliforms and E. coli, identification to the
species level or analyses for other indicator organisms may be undertaken to investigate
the nature of the contamination. Sanitary inspections will also be needed.

Faecal streptococci
Faecal streptococci are those streptococci generally present in the faeces of humans and
animals. All possess the Lancefield group D antigen. Taxonomically, they belong to the
genera Enterococcus and Streptococcus. The taxonomy of enterococci has recently
undergone important changes, and detailed knowledge of the ecology of many of the new
32
species is lacking; the genus Enterococcus now includes all streptococci that share certain
biochemical properties and have a wide tolerance of adverse growth conditions—E.
avium, E. casseliflavus, E. cecorum, E. durans, E. faecalis, E. faecium, E. gallinarum, E.
hirae, E. malodoratus, E. mundtii, and E. solitarius. Most of these species are of faecal
origin and can generally be regarded as specific indicators of human faecal pollution for
most practical purposes. They may, however, be isolated from the faeces of animals, and
certain species and subspecies, such as E. casseliflavus, E. faecalis var. liquefaciens, E.
malodoratus, and E. solitarius, occur primarily on plant material.
In the genus Streptococcus, only S. bovis and S. equinus possess the group D antigen and
therefore belong to the faecal streptococcus group. They derive mainly from animal
faeces. Faecal streptococci rarely multiply in polluted water, and they are more persistent
than E. coli and coliform bacteria. Their primary
value in water-quality examination is therefore as additional indicators of treatment
efficiency. Moreover, streptococci are highly resistant to drying and may be valuable for
routine control after new mains are laid or distribution systems are repaired, or for
detecting pollution of groundwaters or surface waters by surface
run-off.

Principal analytical techniques

The standardization of methods and laboratory procedures is important. International
standard methods should be evaluated under local conditions before they are formally
adopted by national surveillance programmes. A list of ISO standard methods is given in
the Bibliography. The methods described in the annexes to this publication are based on
these ISO standard methods, modified where appropriate in the light of experience in the
surveillance of community water supplies.
The principal methods used in the isolation of indicator organisms from water are the
membrane-filtration (MF) method, the multiple-tube (MT) or most probable number
(MPN) method and presence–absence tests.

Membrane-filtration method
In the membrane-filtration (MF) method, a minimum volume of 10 ml of the sample (or
dilution of the sample) is introduced aseptically into a sterile or properly disinfected
filtration assembly containing a sterile membrane filter (nominal pore size 0.2 or
0.45m). A vacuum is applied and the sample is drawn
33
through the membrane filter. All indicator organisms are retained on or within the filter,
which is then transferred to a suitable selective culture medium in a Petri dish. Following
a period of resuscitation, during which the bacteria become acclimatized to the new
conditions, the Petri dish is transferred to an incubator at the appropriate selective
temperature where it is incubated for a suitable time to allow the replication of the
indicator organisms. Visually identifiable colonies are formed and counted, and the
results are expressed in numbers of “colonyforming units” (CFU) per 100 ml of original
sample.
This technique is inappropriate for waters with a level of turbidity that would cause the
filter to become blocked before an adequate volume of water had passed through. When it
is necessary to process low sample volumes (less than 10 ml), an adequate volume of
sterile diluent must be used to disperse the sample before filtration and ensure that it
passes evenly across the entire surface of the membrane filter. Membrane filters may be
expensive in some countries. Typical sample volumes for different water types are shown
in Table 4.3.
Where the quality of the water is totally unknown, it may be advisable to test two or more
volumes in order to ensure that the number of colonies on the membrane is in the optimal
range for counting (20–80 colonies per membrane).

Multiple-tube method
The multiple-tube method is also referred to as the most probable number (MPN) method
because—unlike the MF method—it is based on an indirect assessment of microbial
density in the water sample by reference to statistical tables to determine the most
probable number of microorganisms present in the original sample. It is essential for
highly turbid samples that cannot be analysed by membrane filtration. The technique is
used extensively for drinking-water analysis, but it is time-consuming to perform and
requires more equipment, glassware, and consumables than membrane filtration.
However, the multipletube method may be more sensitive than membrane filtration.

34
The multiple-tube method depends on the separate analysis of a number of volumes of the
same sample. Each volume is mixed with culture medium and incubated. The
concentration of microorganisms in the original sample can then be estimated from the
pattern of positive results (the number of tubes showing
growth in each volume series) by means of statistical tables that give the “most probable
number” per 100 ml of the original sample.
The combination of sample volumes for processing is selected according to the type of
water sample or known degree of contamination. Various configurations and tables may
be used; typical volumes and dilutions are summarized in Table 4.4.
Appropriate volumes of water are added aseptically to tubes or other vessels containing
sterile nutrient medium of a concentration that will ensure the mixture corresponds to
single-strength medium. For example, 10 ml of sample would typically be added to 10 ml
of double-strength medium or 1 ml of sample to 10ml of single-strength medium and so
on. The tube must also contain a small inverted glass tube (Durham tube) to facilitate the
detection of gas production. Growth in the medium is confirmed by visible turbidity
and/or a colour change. Tubes are incubated without resuscitation, and the number of
positive reactions is recorded after 24 and/or 48 hours, depending on the type of analysis.

Presence–absence tests
Presence–absence tests may be appropriate for monitoring good-quality drinking- water
where positive results are known to be rare. They are not quantitative and, as their name
suggests, they indicate only the presence or absence of the indicator sought. Such results
are of very little use in countries or situations where contamination is common; the
purpose of analysis is then to determine the degree of contamination rather than indicate

35
whether or not contamination is present. Thus, presence–absence tests are not
recommended for use in the analysis of surface waters, untreated small-community
supplies, or larger water supplies that may experience occasional operational and
maintenance difficulties.

Choice of methods
Very often the choice between the multiple-tube and the membrane-filtration methods
will depend on national or local factors, e.g. the equipment already available or the cost of
certain consumables. The advantages and disadvantages of each method should be
considered when a choice has to be made; these are summarized in Table 4.5. The
schematic decision-making network shown in Fig. 4.3 will aid the selection of procedure
and method. The purpose of this diagram is merely to provide suggestions for the
approach to be used; local or other circumstances will also affect the final decision.

Minimizing the cost of analysis

It is sometimes clear that faecal contamination exists (e.g. immediately downstream of a
sewage discharge) or that contamination is very unlikely (e.g. in a distribution network
with a free chlorine residual greater than 0.5 mg/litre, median turbidity less than 1 NTU,
and pH less than 8.0). Microbiological analysis may then be deemed unnecessary. This is
not appropriate, however, under certain conditions, e.g. where there is a legal requirement
to conduct analysis, or where legal action that may be taken would depend on the results
of a microbiological analysis of the water.
Omission of microbiological analysis under the appropriate conditions mentioned above
may contribute to minimizing costs. It may also ensure that adequate numbers of samples
are investigated overall where the resources available.

36
37
for analysis are inadequate to undertake the recommended number of microbiological
analyses.

38
Laboratory-based versus on-site testing
Water-quality testing in communities may be subject to the following problems,
especially when the communities or the sampling sites are remote or inaccessible:

— deterioration of samples during transport to centralized laboratory facilities;

— high cost of transporting samples;
— inadequate techniques for sample storage and preservation during prolonged
transport, thus limiting the sampling range;
— increased personnel costs because of the need for repeat sampling
journeys;
— the need for reporting, which may necessitate further return journeys.
If there are delays in sample transport and analysis—and therefore in reporting—
remedial action is also likely to be delayed. For these reasons, on-site water
testing using portable equipment is appropriate in many remote areas. Portable equipment
is used in many developing countries, and does help to overcome a number of logistic and
financial constraints. However, it varies widely in technical specifications, including the
range of analyses that can be performed, the range
of methods employed, its robustness, the degree of independence from central laboratory
facilities, its portability, and requirements for consumables. Portable testing equipment
may also be favoured by agencies that undertake project monitoring in more than one area
on a non-routine basis and therefore
prefer portability to the establishment of a conventional laboratory. For reasons that
include the following, portable equipment may also be used in conventional laboratories
in place of normal laboratory equipment, especially when the number of analyses to be
performed per day is relatively low.
• Independence from (unreliable) power supplies. Several types of portable equipment
either incorporate a rechargeable battery or may be connected to an external battery.
Where energy supplies are unreliable (because of either voltage fluctuation or intermittent
supply), battery operation may be
advantageous.

• Cost. Comparison of the costs of the equipment required, even after allowing for that
needed for back-up, may show that it is more economical to provide portable testing

39
equipment to peripheral or decentralized laboratories than conventional laboratory
equipment.
• Ease of use. Because portable equipment is often designed for use by personnel who are
not fully qualified in laboratory techniques, its use is usually straightforward. However,
this does not obviate the need for proper training of personnel, particularly since some
portable equipment may not be accompanied
by clear, well-illustrated manuals in the language of the users.

disadvantages, including limitations in technical specifications. Although not invariably

true, the requirement for portability may mean that portable equipment is of lower
precision and sensitivity than conventional equipment. Moreover, while some types of
portable equipment help to reduce dependence on
expensive consumables that may be difficult to obtain in many countries (e.g. by
employing reusable aluminium Petri dishes, rather than dishes made of disposable plastic
or fragile glass), others actually increase dependence on non-standard glassware and,
particularly, consumables (such as microbiological culture media in ampoules and
preweighed reagents for chemical tests). These items are invariably more expensive than
ordinary laboratory consumables and may be available only from the manufacturer of the
portable equipment. Independence of special consumables is of particular importance for
some reagents and microbiological culture media; ready-prepared liquid media in
ampoules eliminate errors in media preparation but they have only limited shelf-life. This
is an especially relevant consideration in developing countries, where delays in
importation, variability of demand, and problems with transport may seriously reduce the
remaining shelf-life of media. Under these conditions, it is preferable to supply
dehydrated media—ideally in preweighed quantities—with a relatively long shelf-life.
The use of portable testing equipment may be the result of a commitment to the
decentralization of testing facilities. Whether or not this is the case, it generally means
that small numbers of analyses are undertaken at a larger number of sites, which has
important implications for training:
• The number of personnel carrying out analyses will be greater so that the need for
training will be greater.
• The personnel who are to use the equipment (and who are therefore to be trained) will
not be working in the capital city, but in relatively remote areas far from training centres.

40
• These personnel are less likely to have received good initial training in laboratory
techniques.
Thus there is actually a greater need for training when decentralized waterquality testing
is contemplated, which is in contrast to the popular perception of “simplified” portable
testing equipment for which little additional training is required. Many of the benefits
expected from decentralized water-quality testing
and/or on-site analysis are unlikely to be realized unless adequate resources are devoted
to training.

Physicochemical analysis
Chlorine residual
The disinfection of drinking-water supplies constitutes an important barrier against
waterborne diseases. Although various disinfectants may be used, chlorine in one form or
another is the principal disinfecting agent employed in small communities in most
countries.
Chlorine has a number of advantages as a disinfectant, including its relative cheapness,
efficacy, and ease of measurement, both in laboratories and in the field. An important
additional advantage over some other disinfectants is that chlorine leaves a disinfectant
residual that assists in preventing recontamination during distribution, transport, and
household storage of water. The absence of a chlorine residual in the distribution system
may, in certain circumstances, indicate the possibility of post-treatment contamination.
Three types of chlorine residual may be measured: free chlorine (the most reactive
species, i.e. hypochlorous acid and the hypochlorite ion); combined chlorine (less reactive
but more persistent species formed by the reaction of free chlorine species with organic
material and ammonia); and total chlorine (the sum of the free and combined chlorine
residuals). Free chlorine is unstable in aqueous solution, and the chlorine content of water
samples may decrease rapidly, particularly at warm temperatures. Exposure to strong
light or agitation will accelerate the rate of loss of free chlorine. Water samples should
therefore be analysed for free chlorine immediately on sampling and not stored for later
testing. The method recommended for the analysis of chlorine residual in drinkingwater
employs N,N-diethyl-p-phenylenediamine, more commonly referred to as DPD. Methods
in which o-tolidine is employed were formerly recommended, but this substance is a
recognized carcinogen, and the method is inaccurate and

41
should not be used. Analysis using starch–potassium iodide is not specific for free
chlorine, but measures directly the total of free and combined chlorine; the method is not
recommended except in countries where it is impossible to obtain or prepare DPD.
Procedures for the determination of free chlorine residual are described in Annex 9.

It is important to measure pH at the same time as chlorine residual since the efficacy of
disinfection with chlorine is highly pH-dependent: where the pH exceeds 8.0, disinfection
is less effective. To check that the pH is in the optimal in the field using comparators such
as that used for chlorine residual. With some
chlorine comparators, it is possible to measure pH and chlorine residual simultaneously.
Alternatively, portable pH electrodes and meters are available. If these are used in the
laboratory, they must be calibrated against fresh pH standards at least daily; for field use,
they should be calibrated immediately before each test. Results may be inaccurate if the
water has a low buffering capacity. Procedures for measuring pH using a comparator are
described in Annex 10.

Turbidity
Turbidity is important because it affects both the acceptability of water to consumers, and
the selection and efficiency of treatment processes, particularly the efficiency of
disinfection with chlorine since it exerts a chlorine demand and protects microorganisms
and may also stimulate the growth of bacteria.
In all processes in which disinfection is used, the turbidity must always be low—
preferably below 1 NTU or JTU (these units are interchangeable in practice). It is
recommended that, for water to be disinfected, the turbidity should be consistently less
than 5 NTU or JTU and ideally have a median value of less than 1 NTU.

Turbidity may change during sample transit and storage, and should therefore be
measured on site at the time of sampling. This can be done by means of electronic meters
(which are essential for the measurement of turbidities below 5 NTU). For the monitoring
of small-community water supplies, however, high sensitivity is not essential, and visual
methods that employ extinction and are capable of measuring turbidities of 5 NTU and
above are adequate. These rely on robust, low-cost equipment that does not require
batteries and is readily transportable in the field, and are therefore generally preferred.

42
Procedures for measuring turbidity in the field using a simple “turbidity tube” are
described in Annex 10.

Safety
The safety of staff undertaking analytical procedures, both in the field and in the
laboratory, is of the greatest importance. All staff should be trained in safety procedures
relevant to their work. In the laboratory, individual staff members should be authorized to
undertake procedures involving risk of any type only after appropriate training;
unauthorized staff should not be allowed to undertake analyses. All laboratories should
formulate and implement a safety policy that should cover cleaning, disinfection, and the
containment of hazardous substances. Safety equipment such as fire extinguishers, safety
glasses, and first-aid kits should be suitably located, and readily available; they should be
routinely checked and all
staff should be trained in their use.

Literature Review
Total suspended solids
TSS is identified as a conventional pollutant in the U.S. Clean Water Act. TSS was earlier
known as non-filterable residue (NFR). TSS is the dry-weight of particles which are
trapped by a filter having a specified pore size.
To find TSS of a water sample, measured volume of water should be passed through a
pre-weighed filter having a specified pore size, then taking the weight of filter again after
drying to evaporate the water in the filter paper. Filters composed of glass fibres are
typically used for measuring TSS. The dry weight measure of the particulates present in
the water sample is the gain in weight & it is expressed in units derived or calculated
from the volume of filtered water.
Turbidity also tends to measure almost the same quality of water property as TSS, TSS is
more useful as it gives an actual weight of the undissolved material in the sample
provided.
Total Suspended Solids consist of a huge variety of material, for example, decaying plant,
silt and animal matter, sewage & industrial wastes. Water having high concentration of
suspended solids might cause problems for aquatic life & stream health.

43
High Total Suspended Solids in a water body might indicate higher amount of metals,
pesticides, and bacteria present in the water. Higher amount of TSS can also cause
problems for industrial usee, as the solids might clog or scour pipes and machinery.
Few Factors Affecting Total Suspended Solids
 High Flow Rates

 Soil Erosion

 Urban Runoff

 Wastewater and Septic System Effluent

 Decaying Plants and Animals

 Bottom-Feeding Fish

Total Dissolved Solids

A measure of the combined content of all inorganic and organic substances contained in a
liquid in molecular, ionized or micro-granular suspended form is called Total Dissolved
Solids (TDS). The solids should be small enough to survive filtration through a filter
which has two-micrometer (nominal size or smaller) pores. We generally discuss TDS for
freshwater systems only, as salinity consists of some of the ions contributing in the
definition of TDS. The Study of water quality for streams, rivers and lakes is the most
important application of TDS, although TDS is not a primary pollutant, but TDS is used
as an indication of aesthetic characteristics of drinking water and as an indicator of the
presence of a broad array of chemical contaminants.
Agricultural and residential runoff are primary sources for TDS in receiving waters, and
so are leaching of soil contamination and point source water pollution discharge from
industrial plants. Calcium, phosphates, nitrates, sodium, potassium, sulphates and
chloride comprise few of the important chemical constituents. The chemicals might be
cations, anions, molecules or agglomerations on the order of one thousand or fewer
molecules, so long as a soluble micro-granule is formed. Pesticides arising from surface
runoff are more exotic and harmful elements of TDS. Certain naturally occurring total
dissolved solids arise from the weathering and dissolution of rocks and soils.
Gravimetry and conductivity are the two important methods of measuring total dissolved
solids. Gravimetric methods are the more accurate methods and they involve evaporating

44
the liquid solvent and taking the mass of residues left. This is the best method generally,
but it is time-consuming. If inorganic salts are there as the great majority of TDS,
gravimetric methods are more appropriate.
Concentration of dissolved ionized solids in the water is directly related to the electrical
conductivity of water. Ions in the dissolved solids in water generate the ability for that
water to conduct electrical current, which is measured by a TDS meter or conventional
conductivity meter . Conductivity generally provides an approximate value for the TDS
concentration, usually to within ten-percent accuracy.
Hard water has high TDS levels, which might be the reason for scale buildup in filters,
pipes, and valves, reducing performance and adding to the cost of system maintenance.

In aquariums, spas, swimming pools, and reverse osmosis water treatment systems, we
can see these effects . Total dissolved solids are tested frequently in all these applications,
and filtration membranes are also checked just to prevent adverse effects.
TDS is generally monitored in order to create a water quality environment which is
favorable for organism productivity in the case of hydroponics and aquaculture. For
freshwater oysters, trouts, and other high value seafood, highest productivity and
economic returns are achieved by mimicking the pH and TDS levels of native
environment of each & every species. Total dissolved solids is considered one of the best
indices of nutrient availability for the aquatic plants being grown for hydroponic uses.

Significance of Total Dissolved Solids in Water

The total dissolved solids concentration of good & palatable drinking water should not be
more than 500 mg/L according to general belief. However, higher concentrations might
be consumed without harmful physiological effects and might be even more beneficial
indeed. This limit was set on the basis of taste thresholds. Wildlife and livestock might
get injured by drinking water that contains total dissolved solids exceeding this limit.
Continuous use of such water might cause weakness, scouring, reduced production, bone
degeneration and death. However, temporarily, animals can drink high saline waters, but
that will be harmful if used continuously.

45
Conductivity
The measure of the ability of an electrolyte solution to conduct electricity is called its
conductivity. Conductivity is also referred to as specific conductance. The SI unit of
conductivity is siemens per meter (S/m).
In many industrial and environmental applications, conductivity measurements are used
as an inexpensive, reliable and fast way of getting the measure of the ionic content in a
solution. For example. A typical way to monitor and continuously trend the performance
of water purification systems is the measurement of product conductivity.
Conductivity is directly linked to the the total dissolved solids (T.D.S.) in various cases.
Conductivity is found out by measuring the AC resistance of the solution between two
electrodes. Dilute solutions follow Kohlrausch's Laws of concentration dependence and
additivity of ionic contributions. A theoretical explanation of Kohlrausch's law by
extending the Debye–Hückel theory was given by Lars Onsager.

Units
Siemens per metre id the SI unit of conductivity and it generally refers to 25 °C. Often,
the traditional unit of μS/cm is used in industries. 106 μS/cm = 103 mS/cm = 1 S/cm.
Sometimes, a unit of "EC" (electrical conductivity) is seen on the scales of instruments: 1
EC = 1 mS/cm. Occasionally, we also encounter is a so-called mho (reciprocal of ohm): 1
mho/m = 1 S/m. Historically, mhos antedate Siemens by many decades; good vacuum-
tube testers, for instance, gave transconductance readings in micromhos.
The standard cell, which is most commonly used has a width of 10 mm, and thus for very
pure water in equilibrium with air would have a resistance of about 106 ohm, known as a
megohm, also sometimes known as "megaohm". Ultra-pure water can get to 18 megohms
or more. Thus megohm-cm was used earlier, sometimes spelled as "megohm".
Occasionally, a conductivity is given just in "microSiemens" (removing the distance term
in the unit). While this can be seen as an error, it can generally be assumed to be equal to
the traditional μS/cm. The typical conversion of conductivity to the total dissolved solids
is done assuming that the solid is sodium chloride: 1 μS/cm is taken to be an equivalent of
about 0.6 mg of NaCl per kg of water.
Molar conductivity’s SI unit is S m2 mol−1. Older publications have the unit Ω−1 cm2
mol−1.
The presence of inorganic dissolved solids such as chloride, nitrate, sulfate, and
phosphate anions (ions that carry a negative charge) or sodium, magnesium, calcium,
46
iron, and aluminum cations (ions that carry a positive charge) affect the value of
conductivity in water. Various organic compounds like phenol, oil, sugar and alcohol do
not conduct electrical current well and therefore possess a low conductivity in water.
Temperature affects the conductivity as well: the warmer the water, the higher the
conductivity. For this reason, conductivity is often reported as conductivity at 298.15 K.
Conductivity of water in streams and rivers is affected basically by the geology of the
area through which the water is flowing. Streams running through areas with granite
bedrock generally have lower conductivity because granite is composed of more inert
materials that do not ionize (dissolve into ionic components) when washed into the water.
On the other hand, streams that run through areas with clay soils tend to have higher
conductivity because of the presence of materials that ionize when washed into the water.
Ground water inflows can have the same effects depending on the bedrock they flow
through.
Discharges to streams have the potential to change the conductivity depending on their
make-up. A failing sewage system would raise the conductivity because of the presence
of chloride, phosphate, and nitrate; an oil spill tends to lower the conductivity.
High quality deionized water has a conductivity of about 5.5 μS/m, typical drinking water
in the range of 5-50 mS/m, while sea water about 5 S/m. Distilled water has a
conductivity in the range of 0.5 to 3 μmhos/cm. Studies of inland fresh waters indicate
that streams supporting good mixed fisheries have a range between 150 and 500 μhos/cm.
Conductivity outside this range could indicate that the water is not suitable for certain
species of fish or macroinvertebrates. Industrial waters can range as high as 10,000
μmhos/cm.

Turbidity
The haziness or cloudiness of a fluid due to various individual particles ( TSS or TDS)
that can be seen with naked eyes (like smoke in air) is known as turbidity. The
determination of value of turbidity might be termed as one of the most important tests of
water quality.
Fluids may have suspended solid matter comprising of particles of various different sizes.
While some will be big enough settle down quickly at the bottom of the container if a
liquid sample is left to stand, the smaller ones might settle very slowly or might not settle
at all if the sample is agitated consistently or if the colloidal particles are present. These
solid particles, which are smaller in size are the reason for any liquid to look like turbid.
47
Turbidity (or haze) is considered in the case of transparent solids such as glass as well.
In plastic production, the percentage of light that is deflected more than 2.5° from the
incoming light direction is known as haze.
Turbidity can also be termed as the measure of a liquid’s relative clarity. Turbidity is an
optical characteristic of water and is also an expression of the amount of light scattered by
material in the water when a light shines through the water sample. The higher the
intensity of scattered light, the higher the turbidity. Material causing water to be turbid
include silt, clay, finely divided inorganic and organic matter, soluble colored organic
compounds, algae, plankton and various other microscopic organisms.
Turbidity makes water cloudy or opaque. The water collected in the bottle is used to find
out the turbidity, which is measured by shining a light through the water and is measured
in nephelometric turbidity units (NTU). During periods of low flow (base flow), many
rivers are a clear green color, and turbidities are low, usually less than 10 NTU.

Turbidity and water quality

High concentrations of particulate matter affect light penetration and productivity,
recreational values, and habitat quality, and cause lakes to fill in faster. In streams,
increased sedimentation and siltation can take place, which might result in harming the
habitat areas for fish and other aquatic life. Particles also provide attachment places for
some other pollutants, especially bacteria and metals. That’s why, turbidity readings are
used as an indicator of potential pollution in a water body.

Turbidity and human health

Excessive turbidity, or cloudiness, in drinking water is aesthetically unappealing, and may
also represent a health concern. Turbidity can provide shelter and food for pathogens.
Regrowth of pathogens in the distribution system is promoted if the turbidity is not
removed, leading to waterborne disease outbreaks, which have caused significant cases of
gastroenteritis throughout the world. Although turbidity is not a direct indicator of health
risk, numerous studies show a strong relationship between removal of turbidity and
removal of protozoa. The particles of turbidity provide "shelter" for microbes by reducing
their exposure to attack by disinfectants. Microbial attachment to particulate material has
been considered to aid in microbe survival. Fortunately, traditional water treatment
processes have the ability to effectively remove turbidity when operated properly.

48
pH Value
pH is basically a measure of the acidity or basicity of an aqueous solution. Solutions
having pH less equal to 7.
Primary pH standard values are found out by using a concentration cell with transference,
simply by measuring the potential difference between a standard electrode such as the
silver chloride electrode & hydrogen electrode. Measurement of pH for aqueous solutions
can be done with a pH meter or a glass electrode. We can also find the value of pH by
using indicators.
pH measurements have significant importance in the field of biology, environmental
science, chemistry, medicine, oceanography, food science, agriculture, nutrition ,civil
engineering, chemical engineering, forestry, water treatment & water purification and
many other applications.
Mathematically, it can be said that pH is the negative logarithm of the activity of the
hydrogen ion.

Importance of pH
The solubility (amount that can be dissolved in the water) and biological availability
(amount that can be utilized by aquatic life) of chemical constituents such as nutrients
(phosphorus, nitrogen, and carbon) and heavy metals (lead, copper, cadmium, etc.) can be
determined by pH of water. For example, in addition to affecting how much and what
form of phosphorus is most abundant in the water, pH also determines whether aquatic
life can use it. Metals are generally more toxic at lower pH as they are more soluble.
Extremely low and high pHs can be significant for the use of water. High pH causes a
bitter taste, water pipes and water-using appliances become encrusted with deposits, and
it also depresses the effectiveness of the disinfection of chlorine, thereby generating the
need for additional chlorine when pH is a bit high. Low-pH water might corrode or
dissolve metals and other substances.
Pollution has the potential to change a the pH of water, which might harm animals and
plants living in the water.

Effects on Laboratory Animals

If pH is more than 10, skin irritation might be observed in some of the animals. For
rabbit, this can be observed at a pH of about 9 as well. And if the pH is more tha 10, it

49
might behave as an irritant for the eyes of rabbit . But for a pH less than 5, no significant
effects on eyes were observed.

Effects on Humans
If human beings are exposed to extreme pH values, it might cause irritation to the eyes,
skin, and mucous membranes. Eye irritation and exacerbation of skin disorders have been
associated with pH values greater than 11. In addition, solutions of pH 10–12.5 are said to
cause hair fibres to swell. In sensitive individuals, gastrointestinal irritation may also
occur. Exposure to low pH values can also result in similar effects.

Sulphate Content
Naturally, sulphates are found in various minerals, such as epsomite
(MgSO4·7H2O),gypsum (CaSO4·2H2O) & barite (BaSO4). Such dissolved minerals
constitute the mineral content in drinking water. Sulfates find their way into water
through smelters and mines and also from kraft pulp and paper mills, tanneries & textile
mills. Sulphates of potassium, magnesium and sodium are highly soluble in water, while
barium and calcium sulfates and various other heavy metal sulfates are little less soluble.
Suphur di oxide & Sulphur tri oxide also contribute to the sulphate content of water to
some extent.

Effects on Humans
Cathartic effects are commonly reported to be experienced by people consuming
drinking-water containing sulfate with higher concentraions. Although it is also reported
that humans can adapt to higher concentrations with time .Dehydration is another
common side-effect following the ingestion of large amounts of sodium or magnesium
sulfate exposed to tap water containing sulfate with a median concentration of 264
mg/litre and a range of up to 2787 mg/litre, compared with the risks for those not using
tap water or using low-sulfate tap water, there was no significant association between
sulfate ingestion and the incidence of diarrhoea for the range of concentrations studied.
Reviews of the literature and a study to experimentally determine a
sulfate dose that would induce effects in adults concluded that it was not possible to set a
health-based standard for sulfate in drinking-water and confirmed the conclusions of
other workers.

50
The presence of sulfate in drinking-water can also result in a noticeable mg/litre as the
sodium salt. Sulphate may also contribute to the corrosion of distribution systems.
In the light of the above considerations, no health-based guideline value for sulfate in
drinking water is proposed. However, there is an increasing likelihood of complaints
arising from a noticeable taste as concentrations in water increase above 500 mg/litre.

Chloride Content
Naturally, chlorides are found as salts such as sodium chloride (NaCl), potassium chloride
(KCl), and calcium chloride (CaCl2). Chlorides are leached from different rocks into soil
and water due to weathering. The chloride ion is generally mobile and is shifted to oceans
or closed basins. It is found that chloride concentration in groundwater and drinking-
water is consistently increasing, but there have been a few exceptions. Chloride levels in
unpolluted waters are generally below 10 mg/litre and sometimes even below 1 mg/litre.
Chloride in water may be significantly increased by treatment processes in which chlorine
or chloride is used.

Effects on Humans
Chloride toxicity has not been observed in humans except in the exceptional case of
impaired sodium chloride metabolism. Healthy human beings can tolerate the intake of
large quantities of chloride if there is a sufficient intake of fresh water. Chloride increases
the electrical conductivity of water and also its corrosivity. Chloride concentrations in
excess of about 250 mg/litre can give rise to detectable taste in water, but the threshold
depends upon the associated cations. Consumers can, however, become accustomed to
concentrations in excess of 250 mg/litre. No health-based guideline value is proposed for
chloride in drinking-water.

Iron content in water

Iron accounts for almost 5% in the earth’s crust & is consequently the 2nd most abundant
metal in the earth’s crust. The ions of iron form sulphates, nitrates, carbonates &
hydroxides & elemental iron is rarely found in nature. The most common form of iron
found in nature is that of oxides.
Bacterial growth is generally promoted by iron which is pretty undesirable.

51
Aeration of iron containing layers in soil can affect the quality of both groundwater &
surface water, if the groundwater table is lowered or nitrate leaching takes place.
Dissolution of iron might take place as a result of oxidation & decrease in pH.
The concentration of iron is about 0.7 mg/l in rivers. Concentration is in the range of 0.5-
10 mg/l in anaerobic groundwater where iron is generally in the form of Fe(II).
Conentration of iron in drinking water should be less than 0.3 mg/l.

Manganese content in water

Manganese can be termed as a metal which is one of the most abundant on earth. Though
it is not found in its natural form, it is actually a component of more than 100 minerals.
Manganese can exist in 11 oxidative states.
Manganese occurs naturally in many surface water and groundwater sources and in soils
that may erode into these waters. However, human activities are also responsible for
much of the manganese contamination in water in some areas.
Ambient manganese concentrations in seawater have been reported to range from 0.4 to
10 μg/l , with an average of about 2 μg/l. Levels in fresh water typically range from 1 to
200 μg/l. Manganese has a median level of 16 μg/l in surface waters. Higher levels in
aerobic waters are usually associated with industrial pollution.

Experimental Procedures
Total Suspended Solids
Theory
The solids which can’t survive the filtration through a filter with 2 micrometer pores are
called TSS. And hence, we use that procedure to find TSS.

Apparatus Required
1. Funnel
2. Conical Flask
3. Filter paper
4. Oven
5. Weighing Machine
6. Measuring Cylinder
7. Beaker

52
Procedure
 10 ml of water sample is measured using the measuring cylinder.

 Water sample is transferred into a beaker.

 Weight of the filter paper is recorded.

 Filter paper is adjusted in the funnel.

 Water is transferred to the conical flask through the filter paper.

 Filter paper is kept in the oven in order to get it dried.

 Once the filter paper gets dried, it is taken out.

 The weight of filter paper is then recorded.

 The initial weight of the filter paper is then subtracted from the final weight.

 The result which we get is the amount of suspended solids in 10 ml of water.

 It is divided by 10 in order to get the amount of TSS per ml of water.

Total Dissolved Solids

Theory
The definition of TDS says that the dissolved solids which are small enough to survive
filtration through a filter with two micrometer pores are TDS. And that is the procedure
used here. The water is evaporated after the filtration & TDS is measured.

Apparatus Required
1. Conical flask

2. Petridish

3. Oven

4. Weighing machine

53
Procedure
 TDS is measured in continuation to the procedure of finding TSS.

 A petridish is taken.

 Weight of the petridish is recorded.

 Filtered water from the TSS process is transferred into the petridish.

 Petridish is then kept in the oven.

 The temperature of the oven is set at over 100° C.

 After sometime, water is evaporated.

 The petridish is then taken out.

 The weight of petridish is then recorded.

 The initial weight of the petridish is then subtracted from the final weight.

 The result which we get is the amount of dissolved solids in 10 ml of water.

 It is divided by 10 in order to get the amount of TDS per ml of water.

3.3 pH value
Apparatus Required
1. pH meter

2. Beaker

Procedure
 All the samples are taken in the beaker one by one.

 The pH value is recorded for all the sample using the pH meter.

3.4 Conductivity Apparatus Required

1. Conductivity meter
2. Potassium Chloride (KCl)
3. Small Beaker
4. Distilled Water

54
Procedure
 First, some amount of Potassium Chloride is taken.

 Then, KCl is dissolved in distilled water & the potassium chloride solution is prepared.

 Conductivity of KCl is checked using conductivity meter.

 If there is some error in the conductivity of KCl, then the settings of the conductivity
meter is adjusted accrordingly.

 Then, the sample is taken in the beaker.

 The conductivity of the sample is measured.

 The same procedure is repeated for all the samples.

 Hence, the conductivity of all the samples are recorded.

3.5 Turbidity
Apparatus Required
1. Turbidity meter

2. Distilled Water

3. Beaker

Procedure
 First, the beaker is taken & is washed properly.

 Then, distilled water is poured into the beaker.

 Turbidity of distilled water is measured by the turbidity meter.

55
 If the turbidity is not zero, then the settings are adjusted as to make it zero.

 Then, the beaker is again washed properly.

 Then, the sample is poured into the beaker.

 The turbidity of the beaker is measured using the turbidity meter.

 The same procedure is repeated for all the samples.

3.6 Chloride content in water

Theory
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 AgNO3 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.
Chemicals Required
1. Potassium Chromate

2. Phenolphthalein Indicator

3. Sodium Chloride

4. Silver Nitrate

56
Apparatus Required
1. Conical Flask

2. Standard Flask
3. Beaker

4. Burette

5. Pipette

6. Wash Bottle

Procedure
First, a standard NaCl solution is prepared.

 1.648 g of NaCl is measured.

 NaCl is dissolved in distilled water.

 Volume is made upto 100 ml.

 Solution is transferred to a 100 ml standard flask.

Then, a standard silver nitrate solution is prepared.

 4.791 g of Silver Nitrate is dissolved in distilled water & the volume is made upto 100
ml.

 This solution is standardized against the NaCl Solution.

Then, the potassium chromate indicator is prepared.
 25 g of Potassium Chromate is taken & is transferred to the beaker containing distilled
water.

 Few drops of silver nitrate solution is added until slight red precipitate is formed.

 It is allowed to stand for 12 hrs & then, it is filtered.

 The filtrate is diluted to 1000 ml

 20 ml of sample is taken in a 250 ml flask.

 1 ml of the indicator is added to get a slight yellow colour.

57
 The sample is titrated against the silver nitrate solution until a brick red colour is
observed.

3.7 Sulphate content in water

Theory
The turbidimetric method of measuring sulphates is based upon the fact that barium
sulphate tends to precipitate in a colloidal form of uniform size and that this tendency is
enhanced in presence of sodium chloride, hydrochloric acid and glycerol. The absorbance
of the barium sulphate formed is measured by a spectrophotometer at 420 nm and the
sulphate ion concentration is determined by comparison of the reading with a standard
curve.

Chemicals Required
1. Con. HCl

2. Sodium Chloride

3. Ethyl Alcohol

4. Sodium Sulphate

5. Barium Chloride

6. Glycerol

7. Distilled Water

Apparatus Required
1. Sample Tubes

2. Standard Flask

3. Beaker

4. Measuring Cylinder

5. Tissue Paper

6. UV-visible Sprectrophotometer

58
Procedure
First, a conditional reagent is prepared in the following way.-
 25 ml of glycerol is taken & is poured into a beaker.

 15 ml of con. HCl is added to the same beaker.

 Then, 50 ml of ethanol is added to the same beaker.

 Then, 37.5 g of NaCl is dissolved in distilled water & is added to the beaker.

 The total volume is made to 250 ml.

After preparing the conditional reagent, the sodium sulphate solutions of different
concentrations of 50 ml volume are prepared-
 Blank Solution

 0.2 g/l

 0.4 g/l

 0.6 g/l

 0.8 g/l
50 ml of all the the three samples are also taken.
 Then, 5 ml of reagent is added to all the solutions.

 A pinch of barium chloride is added to all the solutions.

 Then, the absorbance of all the samples is taken using the spectrophotometer at 420
nm.

 A graph is plotted between the absorbance & the concentration of the solution.

 The sulphate content of the samples are found out using the graph.

59
3.8 Iron content in water
Apparatus required
1. Beaker

2. Spectrophotometer

3. Weighing machine

4. Measuring cylinder

Chemicals required
1. Phenanthroline

2. Hydroxylamine hydrochloride

3. Distilled water

4. Iron solution
Procedure
 An iron solution having a concentration of 0.125 g/l was taken.

 Using the solution 6 solutions of different concentration (20 ml each) were prepared. –

1. Blank solution

2. 0.025 g/l

3. 0.05 g/l

4. 0.075 g/l

5. 0.1 g/l

6. 0.125 g/l

 Apart from these six solutions, 20 ml of each sample was taken.

 Phenanthroline & Hydroxylamine hydrochloride were added to all the solutions.

 Absorbances of all the solutions were measured using spectrophotometer at 510 nm.

 A graph was plotted & the concentration of all the samples were determined.

60
3.9 Manganese content in water
Apparatus required
1. Beaker

2. Volumetric flask

3. Measuring cylinder

4. Spectrophotometer

Chemicals required
1. Potassium permanganate

2. Distilled water

3. Conc. Hcl

4. Nitric Acid

5. Sodium Bismuthate

Procedure

 1 mg of pure Mn was dissolved in 2 ml conc. HCl & then diluted to 100 ml using
distilled water.

 From this solution, different solutions of 0.2, 0.4, 0.6 & 0.8 mg/l were prepared & 5
drops of Nitric acid were added to all of them.

 0.01 mg of sodium bismuthate was added to all the solutions.

 Same was done to the samples as well.

 The solutions were bolied for 45 minutes until effervescence was ceased.

 The spectrophotometer was turned on at 510 nm & the absorbances were recorded for
all the samples.

 A graph was plotted & the concentrations of the samples were determined.

61
 Membrane filtration
Membrane filtration is a technique for the separation of suspended or dissolved materials
by molecular weight and size. Application of a pressure differential causes the membrane
to act like a sieve. Substances which are smaller than the pore size of the membrane pass
with the solvent as permeate while larger solutes or particles are retained as concentrate.

 Low Pressure DAF

Dense, homogeneous micro-bubbles generate extremely high interphases and enable in
most cases, a separation of almost 99% of the settleable matters or oil. At the same time,
the systems attain extremely high dry mass contents or pure oil sludge.The Low Pressure
Dissolved Air Flotation (DAF) system’s simple and innovative design increases the flow
by removing effluent from the same end of the tank as the influent is introduced, resulting
in a higher hydraulic loading rate.

Advantages of using Low pressure DAF

 Low energy required.

 Low maintenance efforts.

 High quality industrial components.

 High operational reliability due to self-monitoring systems.

According to Indian Standards : 10500 (Drinking water specifications), the value for TDS
should not be more than 2 g/l. If it exceeds this value, it might cause gastro intestinal
irritation.
However it can also be seen that the value of TDS increases in the month of April as
compared to the values in September. Evaporation & lower flow volume might be the
reason for that. But, the values are much more than the desirable limits.
So, to bring down the value of TDS & to bring the water within the limits of drinking
water specifications, the following measures can be taken.-

62
 Carbon Filters

A method of filtration which uses a bed of activated carbon to remove the impurities &
also the contaminants, using chemical adsorption is called carbon filtering. We get to see
very slight reduction if we use carbon filters.

 Reverse osmosis
Reverse osmosis uses semi-permeable membrane for water purification. This is not a
proper filtration method. Yet, it can be used as it gives high reduction & great tasting
water.

 Distillation
Distillation provides total reduction & flat taste of water. So, it can be used if we want
total reduction.

According to Indian Standards: 10500 (Drinking water specifications), maximum value of

turbidity should be 5 NTU. But here, it is much more than that.
It can also be seen that the value of turbidity is less in April than the value in September.
The reduction in value of TSS might be the reason for that.
The water is certainly not fit for drinking. Few of the steps which might be taken to
reduce the value of turbidity are as follows :

 Cloth filtration
A simple option to pre-treat turbid water is to filter through a locally available cloth.
Users pour water from the transport container through the cloth into the storage container.
The benefits of this option include its simplicity & the wide availability of cloth.

 Sand filtration
Filtration through clean sand is a fast and simple pre-treatment option. Users pour water
from a transport container through a container of sand with gravel and a spigot at the
bottom. The water then flows into a storage container. The benefits of sand filtration are
that it is effective at removing some bacteria, it is simple and fast for the user, and, if sand
is available locally, it is inexpensive. The drawback of sand filtration is that it requires

63
three containers and a spigot. In laboratory studies, the use of sand filtration significantly
reduced both the turbidity and the chlorine demand of turbid water.

 Settling & decanting

Settling and decanting is a method to reduce turbidity by letting the water sit for 2-24
hours so that the particulates settle to the bottom of the container. The clear water is then
decanted off the top into a second container. The benefit of settling and decanting is that
it requires no equipment besides the containers. The drawbacks of settling and decanting
are the need for multiple containers, the time it takes the water to settle, and, if the
containers are opaque, the difficulty in observing the effect of settling. In laboratory
studies, the use of settling and decanting significantly reduced both the turbidity and the
chlorine demand of turbid waters.

Methods used for removal of Iron & Manganese :

Ion exchange
 Conventional water softeners are sometimes effective for removing iron and small
amounts of manganese.

 Softeners are generally only recommended when the water pH is greater than 6.7, the
water hardness is between 3 and 20 grains per gallon (50 to 350 mg/L) and the dissolved
iron concentration is less than 5 mg /L. Oxidized forms of iron and manganese will foul
the softener resin.

 If oxidized iron and/or manganese are present in the raw water, filtration should be
used for removal.

Birm filters
 Birm filters are similar to manganese greensand but they do not require regen.eration
because they utilize oxygen present in the raw water to oxidize the metals.

 As a result, the raw water must contain a certain amount of dissolved oxygen and the
pH should be at least 6.8 for iron removal and 7.5 for manganese removal.

 Even under ideal conditions, manganese removal efficiency is highly variable with
birm filters. Birm filters do require backwashing to remove accumulated oxidized metal
particles.

64
Oxidation followed by filtration
 When combined levels of iron and manganese exceed 10 mg/L, the most effective
treatment involves oxidation followed by filtration.

 In this process, a chemical is added to convert any dissolved iron and manganese into
the solid, oxidized forms that can then be easily filtered from the water. Chlorine is most
commonly used as the oxidant although potassium permanganate and hydrogen peroxide
can also be used.

 A small chemical feed pump is used to feed the chlorine (usually sodium hypochlorite)
solution into the water upstream from a mixing tank or coil of plastic pipe. The mixing
tank or pipe coil is necessary to provide contact time for the iron and manganese
precipitates to form.

 Significant system maintenance is required with these units. Solution tanks must be
routinely refilled and mechanical filters need to be backwashed to remove accumulated
iron and manganese particles.

Conclusion
It can be seen that the amount of total suspended solids has decreased from September,
2013 to April, 2014 in all the three tubewells. The reason might be the dirt particles which
are more significant in the rainy season than in the summer.
As far as the TDS (total dissolved solids) is concerned, the value of TDS increases across
the three samples. Lower flow volume & evaporation might be the reason.
If we take a look at the pH value, it decreases a bit in samples B & C, but is pretty much
constant in sample A.
Conductivity increases in the second set of samples and so is TDS along with that. The
reason being evaporation and lower flow volume again.
Turbidity decreases in the second set of samples. The reason might be the lower TSS.
There is a significant increase in both the sulphate content & chloride content in the
second set of samples. TDS increases and so is the amount of salts dissolved in water.
If we compare the three tubewells, then the water from A seems to be the purest as it is
colourless on both the occasions, is neutral & has the least TSS.
Sample B might be termed as the most impure among the three.

65
Hence, the required properties of all the three samples collected at two different times of
the year were analysed and compared & appropriate measures were suggested wherever
required.

66
References
 American Public Health Association. 1998. "Standard Methods for the Examination of
Water and Wastewater." 20th edition.
 Barber, Larry B. II. 1992. "Hierarchical Analytical Approach to Evaluating the
Transport and Biogeochemical Fate of Organic Compounds in Sewage-Contaminated
Groundwater, Cape Cod, Massachusetts." InGroundwater Contamination and Analysis at
Hazardous Waste Sites, edited by Suzanne Lesage and Richard Jackson. Marcel Dekker,
Inc.
 Caduto, Michael J. 1990. "Pond and Brook." University Press of New England.
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