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GOVERNMENT POLYTECHNIC COLLEGE

MUTTOM

LABORATORY MANUAL
ENVIRONMENTAL ENGINEERING

Name:
Class: Branch:
Roll No: Year:

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2
INDEX
SL Experiment Page no Date Remarks
NO

1 Alkalinity

2 Acidity

3 Hardness

4 Chlorine

5 Residual chlorine

3
4
Date:

INSTRUCTIONS
1. Students shall produce this manual to the practical classes and is to be used as
observation book.
2. Discussions after each experiment should be based on the following points.
a. Limits prescribed for that constituent in drinking water standards/
effluent standards for waste water.
b. The suitability of sample for drinking purpose with respect to the
particular constituent.
3. Students may refer the following for writing discussions.
a. “Standard methods for the examination of Water and Waste Water”-
American Public Health Association, 1015, 18th Street,
N.W. Washington D.C. 20036.
b. “Chemistry for Environmental Engineering”- Sawyer and Mc Caurty,
Tata Mc Graw-Hill.
c. “Manual of standards of quality for drinking water supplies”- Indian
council of medical Research, New Delhi.
d. “International Standards of Drinking Water” – WHO
e. “IS2490-1981,IS3306-1974, IS3307-1977, IS2296-1974, IS10500-
1991” Bureau of Indian Standards, New Delhi, Effluent Standards
KSPCB.

DO’S and DONT’S


1. Do thoroughly clean the glass wares before and after use.
2. Do handle the glass wares carefully.
3. Do not handle chemicals with bare hands.
4. Do not blow out the last drop from the pipette. When the liquid has drained out
completely, touch the tip of the pipette to the inner surface of the vessel.
5. Do not add water to acids. Do always add acid to water.

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6. Do use large volumes of water, when a person is splashed with acid to prevent
serious burns.
7. Do weigh the articles in a balance only at room temperature.
8. Do use different pipettes for different reagents.
9. Do not pipette acids and toxic reagents by mouth.
10. Do read the level of meniscus, in all volumetric glass wares, with the eye at
approximately the same level as the curve of solution.
11. Do clean the workplace and all the glass wares used before leaving the lab.

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1. ALKALINITY
Date: ...........

GENERAL:

The alkalinity of water is a measure of its capacity to neutralise acids. It is


primarily due to the salts of weak acids, although weak or strong bases may also
contribute. Alkalinity is usually imparted by bicarbonates, carbonates and hydroxide.
Bicarbonates represents the major form if alkalinity as they are formed in
considerable amounts from the action of carbon dioxide upon basic materials in the
soil. Other salts of weak acids such as borate, silicates and phosphates may be present
in small amounts. In polluted or anaerobic waters, salts of weak acids such as acetic,
propionic and hydrosulphuric may be produced and would also contribute to
alkalinity. In other cases, ammonia or hydroxide may contribute to the total
alkalinity. Although many materials may contribute to the alkalinity of water, the
major portion of alkalinity in natural water is caused by three major classes of
materials that may be ranked in order of their association with high pH values as
follows: (1) Hydroxide, (2) Carbonates and (3) Bicarbonates. The alkalinity of water
is due to salts of weak acids and strong bases, and such substances act as buffers to
resist a drop in pH resulting from acid addiction. Alkalinity is thus a measure buffer
capacity and in the sense is used to a great extend in waste water treatment practice.
Surface waters where algae grow profusely contain appreciable amounts of
carbonates and hydroxide alkalinity. Alkalinity influences chemical and biological
processes in water and waste water.

AIM:
To determine the amount of the different species of alkalinity viz. Hydroxide
alkalinity, carbonate alkalinity and bicarbonate alkalinity present in the given
samples.

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PRINCIPLE:

Alkalinity is determined by titration with standard solution of a strong acid to


the successive bicarbonate and carbonic acid equivalence points, indicated by means
of colour. For example whose initial pH is above 8.3, the titration is made in two
steps. In the first step the titration is conducted until the pH is lowered to the point at
which phenolphthalein indicator turns from pink to colourless. This corresponds to a
pH about 8.3 by this time all the hydroxide has been neutralised and the carbonate
has been converted into bicarbonate. The second phase of the titration is conducted
until the pH is lowered to about 4.5 corresponding to the methyl orange end point. By
this time all bicarbonates will be converted to carbonic acid. The alkalinity measured
to phenolphthalein end point is known as phenolphthalein alkalinity and the alkalinity
measured up to methyl orange end point represents the total alkalinity.

APPARATUS:
1. Burette 2. Erlenmeyer flasks 3. Pipettes

REAGENTS:

1. Standard sulphuric acid or Hydrochloric acid (0.02 N)


2. Methyl orange indicator
3. Phenolphthalein indicator

PROCEDURE:

1. Pipette 50ml of sample into an Erlenmeyer flask (V)


2. Add 1 drop of sodium thio sulphate solution, if residual chlorine is present
3. Add 2 drops of phenolphthalein indicator. If the pH is above 8.3, colour of the
solution becomes pink.
4. Titrate the sample against standard 0.02 N acid in the burette till the colour just
disappears. Note the volume of titrant used (V1).
5. Then add two drops of methyl orange indicator. The colour turns to yellow.
6. Again titrate the acid till the yellow colour just turns orange yellow.
7. Note down the volume of the titrant used from the initial as (V2).

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CALCULATION:

Phenolphthalein alkalinity as CaCO3 = (V1 x N x 50 x 1000) / V mg/L

Methyl orange alkalinity or total alkalinity as CaCO3 = (V2 x N x 50x 1000) / V

Where , V – Volume of sample used in ml

V1 – Volume of standard acid used up to phenolphthalein end point

N - Normality of acid used

V2 - Volume of standard acid used up to methyl orange end point

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OBSERVATION:

Sample 0.02 N H2SO4 Methyl orange / phenolphthalein indicator

sa Tri Burette reading Volume of acid used Total


mp al alkali
le No nity
Initi At At Initial to Mean Initial to Mean
. (mg/
al phenolphth methyl phenolph vol. methyl vol.
L)
alein end orange thalein (V1) orange (V2)
point end end point (ml) end point (ml)
point
1

2
3
1

2
3

SAMPLE CALCULATION:

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Species of alkalinity may be obtained from the table given below.

Alkalinity relationships

Sl.No. Results of Hydroxide Carbonate Bicarbonate


Titration Alkalinity as Alkalinity as Alkalinity as
CaCO3 CaCO3 CaCO3
1 P=0 0 0 T
2 P<½ T 0 2P T – 2P
3 P=½T 0 2P 0
4 P>½T 2P – T 2(T-P) 0
5 P=T T 0 0

APPLICATION OF ALKALINITY DATA :

Information concerning alkalinity is used in a variety of ways in environmental


engineering practice. In chemical coagulation, alkalinity acts to buffer the water in a pH
range where the coagulant can be effective. Alkalinity must be present in excess of that
destroyed by the coagulant for effective and complete coagulation of water. Alkalinity is a
major item that must be considered in calculating the lime and soda ash requirements in
softening water by precipitation methods. Alkalinity is an important parameter involved in
corrosion control and as a means of evaluating the buffering capacity of wastewaters and
sludge. Alkalinity is an important factor in determining the amenability to wastewater to
biological treatment.

SPECIFICATION:

Potable water:

As per IS 10500: 1991, the desirable limit of alkalinity in potable water is 200 mg/L.
However in absence of any alternate source, the permissible limit shall be 600 mg/l as
CaCO3.

Water for concrete preparation:As per IS 456: 2000, to neutralise 100ml sample of water
using mixed indicator, it should not require more than 25 ml of 0.02 N H2SO4 (ie,
alkalinity < 250 mg/l).

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RESULT:

QUESTIONS

1. Which is the major form of alkalinity? How is it formed?


2. Why do we take 0.02 N H2SO4 for the titration?
3. Why does the pH change on aerating the water?
4. For efficient coagulation, the water must be alkaline. Why?

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2.ACIDITY
Date: ………

GENERAL:

Acidity of water is its quantitative capacity to neutralize a strong base to a designated


pH. Strong mineral acids, weak acids such as carbonic acid and acetic acid and hydrolysis
salt such as ferrous or aluminium sulphate contribute to the measured acidity according to the
method of determination. Acidity contributes corrosiveness to water and influences certain
chemical and biological processes.

AIM:

To determine the acidity of the given sample of water.

PRINCIPLE:

Acidity can measured by titrating the samples with standard solution of alkaline
reagents. Mineral acids are neutralized by titration to a pH of about 4 to 5 or by using methyl
orange as the indicator. Since methyl orange is used as indicator , acidity is also called methyl
orange acidity. Most of the weak acids are neutralized by titration to pH 8.3 and
phenolphthalein is used as the indicator. Titration of sample to the phenolphthalein end point
of pH 8.3 measures both mineral acidity and acidity due to weak acids. This total acidity is
also termed as phenolphthalein acidity. Results are in terms of methyl orange or
phenolphthalein acidity expressed as CaCO3.

APPARATUS:

1. burette

2. Pipettes

3. Erlenmeyer flasks

REAGENTS:

1. 0.02 standard NaoH solution.


2. Methyl orange indicator.

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3. Phenolphthalein indicator.
4. 0.01N Sodium thiosulphate.

PROCEDURE:

1. Pipettes 50 ml of the sample into an Erlenmeyer flask.


2. Add 1 drop of 0.1 N Sodium thiosulphate solution, if residual chlorine is present.
3. Add 2 drops of methyl orange indicator.
4. Titrate the sample against 0.02 N NaoH solution.
5. Note the volume of the titrant at the end point when color changes from orange
red to yellow (V1).
6. Add 3 drops (0.15 ml) of phenolphthalein indicator to the above and continue the
titration to the appearance of faint pink color characteristics of pH 8.3.
7. Note the volume of titrant used (V2).

CALCULATION :

Mineral acidity in mg/l as CaC03 = (V1x N x 50 x 1000)/V

Total acidity in mg/l as CaC03 = (V2 x N x 50 x 1000)/V

Where,

V1= ml of NaOH titrant up to methyl orange end point.

V2= ml of NaOH titrant up to phenolphthalein end point.

N= Normality of NaOH.

V= ml of sample.

APPLICATION OF ACIDITY DATA:

Acidity is of little concern from a sanitary or public health viewpoint. However,


acidity due to carbon dioxide is practically important in the field of public water supplies.
Many underground supplies require treatment to overcome corrosive characteristics resulting
from carbon dioxide. The amount present in an important factor in determining whether
removal by aeration or simple neutralization with lime or NaOH will be chosen as treatment

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OBSERVATION:

0.02 NaOH x sample Methyl orange/ Phenolphthalein


indicator

Sa Trial Burette reading Volume of titrant used


mp No Initial At At Initial to Mean Initial to Mean To
le methyl phenolph Methyl Vol.(V1) phenolph vol. tal
orange thalein orange (ml) thalein (V2) aci
end end point End Point end point (ml) dit
point pH- 8.3 y
pH- 4.5 (m
g/
L)
1
2
3
1
2
3

Sample calculation:

method. Most industrial wastes containing mineral acidity must be neutralized before
they may be discharging into rivers or sewers or subjected to treatment of any kind.

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SPECIFICATIONS:

Potable water:

No range of acidity is specified, as the mineral acidity is restricted indirectly by the


stipulation of Ph in range 6.5-8.5.

RESULT:

INFERENCE:

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3.HARDNESS
Date:..............

GENERAL:

Hardness is caused by divalent metallic cations. Such ions are capable of reacting
with soap to form precipitates and with certain anions present in the water to form scale in
hot water pipes, heaters, boilers etc. The principle hardness causing cations are calcium,
magnesium, strontium, ferrous iron manganese ions.

Principle cations causing hardness in water and the major anions


associated with them are given in the table below:

Cations causing hardness Anions


Ca2+ HCO3-
Mg2+ SO4-
Sr2+ Cl-
Fe2+ NO3-
Mn2+ SiO3

AIM:

To determine the total hardness of the given sample of water and hence to estimate the
carbonate and non-carbonate hardness of the same sample.

PRINCIPLE:

EDTA Titrimetric method

Solution of EDTA (Ethylene Dyamine Tetra Acetic Acid) or its sodium salt is used as
the titrating agent. EDTA forms extremely stable complex ions with Ca2+, Mg2+ and other
divalent cations causing hardness.

Mg2+ EDTA -------------- (MEDTA) Complex

Eichrome black T is used as indicator. when a small amount of Erichrome black T,


having a blue colour, is added to the hard water with a pH of about 10, it combines with a few
of the Ca2+ Mg2+ ions to form a weak complex ion which is wine red in colour.

Mg2+ + Erichrome black T → (M Erichrome black T) complex

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During titration with EDTA, all free hardness ions are complex according to equation (1).
Finally EDTA disrupts the (M Erichrome black T) complex and frees the Erichrome black T
indicator and the wine red colour changes to blue, marking the end of the titration.

APPARATUS:

1. Burette 2. Pipettes 3. Erlenmeyer flasks

REAGENTS:

1. Ammonia buffer solution


2. Enrichrome Black T in dicator
3. Standard EDTA titrant 0.01 M

PROCEDURE:

1.Take a sample volume which will require less than 15 ml EDTA titrant.

2. Dilute 25 ml of sample to about 50 ml by adding distilled water (V).In case of sample of


with low hardness take a larger sample volume.

3. Add one or two ml of buffer solution to bring the pH to 10 ± 0.1.

4. Add one or two drops of indicator solution. If Ca or Mg hardness is present, the solution
will turn wine red.

5. Titrate against EDTA titrant till the sample turns blue. Note the volume Vl of the titrant .

CALCULATIONS:

Hardness as CaCO3 = Vl x S x 1000 mg/L

Where,

V1= volume in ml of titrant used for the sample

S (mg of CaCO3 equivalent to 1 ml of EDTA titrant ) = 1 (mg CaCO3)

V = Sample volume

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OBSERVATIONS:

Sample x EDTA Erichrome Black T indicator

Description Trial Volume Burette Volume of Mean volume HardnesMg/L


of sample No. of reading EDTA(ml) of as CaCO3
sample EDTA(VlmL)
(VmL) initial Final
1
2
3
1
2
3

Sample calculation: Sample No:

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If carbonate and bicarbonate alkalinity is greater than total hardness,

Carbonate hardness = Total hardness

Non carbonate hardness =0

If carbonate and biocarbonate alkalinity , is less than total hardness,

Carbonate hardness = alkalinity

Non carbonate hardness = Total hardness – alkalinity

Application of hardness data:

Hardness of water is an important consideration in determining the suitability of


water for domestic and industrial uses. It is used as a basis for recommending the need for
domestic process. The relative amounts of calcium and magnesium hardness and carbonate
and non carbonate hardness present in water are factors in determining the most economical
types of softening process to use.

Water commonly classified in terms of degree of hardness, as follows :

Hardness in mg/l Degree of hardness

0-75 Soft
75-150 Moderately hard
150-300 Hard
>300 Very hard

Specifications:

IS 10500:1991 specifies desirable limit of hardness as 300mg/l in potable water and rejection
limit as 600mg/l of CaCO3.

For boiler feed water the hardness should not be greater than 10mg/l as per IS10392: 1982.

Hardness may vary from zero to a few hundreds of mg/l depending on the source and the
treatment to which the water has been subjected.

RESULT:

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4.CHLORIDES

Date:........................
GENERAL:

Chlorides in the form of CF ions is one of the major anions in water. In potable water
salt content is produced by the chlorides. Water having 250mg/L chloride may have a salty
taste if the cation is sodium. On the other hand, a typical salty taste will be absent even in
water containing as much as 1000mg/L chloride, if the predominant cations are Ca and Mg.
Chloride concentration is higher in wastewater than in raw water because sodium chloride is
discharged through urine and excreta. So the presence of chlorine in water indicates the
possibility of contamination of water by sewage. High chloride contents are harmful to
metallic pipes and agricultural crops.

AIM:

To determine the chloride content present in the given water samples.

PRINCIPLE:

Chloride can be determined either by Mohr’s method (argentometric) or by mercuric


nitrate method of which former is described here. The method employs solution of silver
nitrate(N/71).This correspond to a solution of N/71 or one of which each ml is equal to 0.5mg
of chloride ion is prescribed as a white silver chloride.

Ag+ + Cl- ↔ AgCl

The end point cannot be detected by eye unless and indicator capable of
demonstrating the presence of excess Ag+ is present. The indicator used is potassium
chromate, which supplies the chromate ions .As the concentration of chloride ions approaches
extinction ,the silver ion concentration increases to a level at which the solubility product of
silver chromate is exceeded and it begins to form a reddish brown precipitate.

2Ag++ + CrO42- ↔ Ag2CrO4 (reddish brown ppt)

Since excess amount of Ag ion is needed to produce visible amount of Ag2 CrO4 the
indicator blank must be determined and subtracted from all the titration. In a neutral or a salty
alkaline solution, potassium chromate can indicate end point of silver nitrate titration of
chloride. Silver chloride is precipitated quantitatively before red colour silver chromate is
formed.

APPARATUS:

1.Burette 2.Pipettes 3.Erlenmeyer flask

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REAGENTS:

1.Chloride free distilled water

2.Potassium chromate indicator solution

3.Standard silver nitrate solution (0.0141N)

4.Aluminium hydroxide suspension

5.Hydrogen peroxide

6.H2 SO4/ NaOH

PROCEDURE:

1.Take 100mL of sample (v)or a suitable portion diluted to 100mL.

2.If the sample is coloured, add 3mL of aluminium hydroxide suspension ,mix, allow to
settle, filter, wash and collect the filtrate.

3.If sulphide, sulphite or thiosulphate is present ,add 1mL of hydrogen peroxide and stir for 1
minute.

4.Bring this sample to a pH range of 7 to 10 by adding H2SO4 or NaOH as required.

5.Add 1mL of potassium chromate indicator solution.

6.Titrate this against standard silver nitrate titrant to brick red end point. Note the volume
(V1)

7.Repeate the procedure using blank (distilled water and note the volume (V2)

CALCULATIONS:

Chlorides in mg/L = (V1 –V2) x N x 35.45 x 1000

Where, V1 = Volume of titrant for sample in mL

V2 =Volume of titrant for blank in mL

N =Normality of silver nitrate solution

V =Volume of sample in mL

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Observation

Sample x 0.01
Sample Trial Volume of Burette reading Volume of Mean Chloride
No No the sample titrant(mL) volume v1 (mg/L)
(mL) Initial Final (mL)

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APPLICATION OF CHLORIDE DATA:

In many areas the level of chloride in natural water is an important consideration in


the selection of supplies for human use, where brackish water must be used for domestic
purpose ,the amount of chlorides present is an important factor in determining the type of
desalting apparatus to be used. The chloride determination is used to control pumping of
ground water from location where intrusion of sea water is a problem. Chlorides also
interfere in the determination of COD.

SPECIFICATIONS:

IS 10500-1991 specifies the desirable limit of chloride content as 250mg/L and


permissible limits as 1000mg/L in case of absence of alternate source. The chloride content is
limited to 500mg/L for RCC work and 2000mg/L for concrete not containing steel as per IS
456-2000.

RESULTS AND DISCUSSIONS:

INFERENCE:

QUESTIONS:

1.Explain the significance of high chloride concentration in water supplies.

2.What are the sources of chloride in water?

3.Explain the need for blank correction.

4.Why must the pH of the sample be neither high nor low?

5.Why the normality of silver nitrate is taken as 0.0141 N ?

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5.RESIDUAL CHLORINE

Date :

GENERAL :

Chlorination is done to destroy pathogense and to reduce the effects of iron,


manganese, sulphide and organic substance. Chlorination produces characteristic tastes
when;traces of phenols are present and when algae are present pungent odours are produced.
To promote the purpose of chlorination , is essential that a residual is maintained in the water
This residual chlorine must be tested in a routine analysis. The destruction of micro
organisam is a primary fuction of chlorination so as to prevent water born diseases . Overall
improvement in the finished water can result from chlorine’s reaction with ammonia, iron,
manganese and sulphide and protein substances. Chlorine in water may be present as a free
available chlorine (in the form of hypochlorous acid or hypochlorite ion); as combined
available chlorine(chloramines and other derivatives).Several tests like orthotoludine test,
idometric method etc can used to determine residual chlorine in water.Idometric method is
more precise than colourimetric method (or orthotoludine test) where residual concentration
exceeds 1mg/l, but for lower concentration it is not so accurate.

AIM :

To determine the amount of residual chlorine in the given sample by starch iodide
method.

PRINCIPLE :

Chlorine will liberate free iodine from potassium iodide solution at pH 8 or less.
The libarated iodine is titrated against standard. Sodium thiosulphate with starch as indicator.
The reaction is preferably carried out at pH 3-4. The minimum dectetable concentration must
be 40 of Cl , if 0.001 N sodium thiosulphate is used with 500 ml sample.

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APPARATUS :

1. Burette 2. Pipetts 3. Erlenmeyerflask (1L)

REAGENTS :

1. Acetic acid concentrated


2. Pottasium iodide
3. Standard sodium thiosulphate 0.01 N
4. Starch indicator solution
5. Standard iodine

PROCEDURE :

1. Take 5 ml of Acetic acid in 1L Erlenmeyer.

2. Add about 0.05 gm of Kl to this (estimated on spatula).

3. Pour 500 ml sample into the flask and mix well with stirring rod.

4. Titrate this mixture against 0.01 N sodium thiosulphate in a burette until the colour if the

Sample is yellow.

5. At this stageadd 1 ml of starch solution and then the colour become blue.

6. Continue titration till the blue colour just disappears. Note the volume(V1).

7. Blank titration.

8. For blank titration, prepare 500 ml of distilled water as sample for titration and add 1 ml
of starch solution to it, and 5 ml of acetic acid and 0.05 gm

9. If blue colour develops, titrate with 0.01 N sodium thiosulphate till blue colour disappears.

Note this volume of titrant ads negative (V2).

10. If no blue colour occur, titrate with 0.0282 N (N/35.45) iodine solution until blue colour

appears. Black titrate with 0.01 N sodium thiosulphate and record thr difference as

positive V2

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OBSERVATIONS
Sample x 0.01 N Sodium thiosulphate starch indicator

Sample Trial Volume of Burette reading Volume of Mean Chloride


No No the sample titrant(mL) volume v1 (mg/L)
(mL) Initial Final (mL)

Sample calculation:

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CALCULATIONS :

Residual chlorine = (V1 ± V2) x N x 35.45 x 1000 / V

Where ,

V = Volume of sample in ml

V1 = ml of titrant for sample

V2 = ml of titrant for blank

N = normality of sodium thiosulphate

Note : Reagent impurities such as

(a) Free iodine in KI that liberates extra iodine.


(b) traces of reducing agents, that may reduce some of the iodine liberated, may be present
and hence blank titration will eliminate such discripancies.

APPLICATION FOR RESIDUAL CHLORINE DATA :

Chlorine residual are used universally in disinfection practice to control addition of


chlorine so as to ensure effective disinfection without the waste of chlorine. They are also
used to control chlorination of domestic industrial wastes and usually are sole criteria
immediately available to determine whether objectives are being attained

RESULT

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