Introduction

Water analysis &

Purification
Prepared by :- Dr.Walaa Adel El-hamdy
 Introduction
Water is the pillar of life. It is the principal chemical
constituent of the body.

It is the most commonly used solvent. It is vital for

drinking, washing, sanitary disposal of wastes, in
irrigation, farming and industrial uses.

Water analysis is characterized by the high dilution of

ingredients, which limits most analytical methods to
the semi-micro and micro scales. Sensitive
colorimetric methods are frequently used. 3
 Water forms about 2/3 (two third) of entire the body
weight
 Importance of water
 1-regulate body temperature
 2- it is responsible for the production of digestive
guises
 Properties of water
 1- it is clear ,transparent ,tasteless and odorless fluid
 2- it is colorless pale blue through deep colum
 - it is freezes at 00C and boils at 100 0C under normal
pressure
 It has great density at 4o C
 It dissolves almost all substances ,solid liquid or gases
Classification of water
 Classification of water according purity
 Classification of water according source
 Classification of water according uses
 According to purity
a- pure water (free of chemical infection disease ,human
and animal waste)
b – polluted water (Type of water undergoes changes in
its physical character Ex,odor and color
C- contaminated water (contains elevated concentration
of substance above neutral level)
 According to source
 a- rain water : it may contain some dissolved gases Ex:
O2,N2,NH3 and nitrous oxide
the presence of CO2 and nitrous oxides causes acidity to
rain water
B- surface water : when rain falls on earth ,it may
collected in lakes or rivers ddissolve salts and minerals,
carries colloidal and suspended particles.
C- Under ground water : dissolves minerals
Physical properties
 1- Color
 2- Odour
 3- Turbidity
 4- Electrical conductivity
 Color
 True color : color of sample due to the presence of soluble
matter
 Apparent color : color of sample as received from its
source due to the presence of soluble and suspended
matter.
 The colour is noted as (colourless, weakly yellowish,
yellowish, yellow, yellowish/brown, brown,
yellowish/green and greenish).
Turbidity
Sources:
inorganic (colloidal rock or soil particles), or organic
materials.
Sanitary significance:
- The acceptable limit is of 5 NTU (National Turbidity Unit).
- Excessive turbidity can protect microorganisms from
disinfection.
- Stimulate the growth of bacteria in the water.
- Filtration is more difficult.
- Disinfection by chlorine or ozone or chlorine is less effective
Determination:
- Jackson Candle Turbidimeter.
- Photoelectric instruments (turbidimeter or nephelometer).
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5. Total and volatile solids (TDS):
Total solids are:
- Suspended (suspended solids, SS).
- Volatile solids (VS) are the fraction of the total solids
burnt off at 600oC while the remaining fraction is the
fixed solids (FS).
Sources:
Inorganic salts and small amounts of organic matter
originating from natural sources, sewage discharge,
or industrial waste.
Sanitary significance
The palatability of drinking water according to the TDS
limits (1200 mg/L).
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Chemical Examination of water
 - Determination of total solids
 2- pH value
 3- Alkalinity
 4- Acidity
 -Chlorides
 - Fluorides
 7- Water hardness and softing
 8- gases dissolved in water
 9- Metals in water
 10- Pollution
 1-purification of water
 Determination of Acidity in water and sewage
 -CO2
 Strong mineral acids as sulphuric acid or HCl
 3- Weak organic acid s such as Carbonic acid ,acetic
acid and tannic acid
 4- Hydrolyzable metals (salts ) such as iron
,aluminum and manganese
 Acidity is usually expressed in term of CO2
 The amount of acidity indicates the water s degree of
corrosiveness
Determination It is determined by titration with
standard solution of strong alkali :
(N/50NaOH) and methyl orange
(mineral acidity) .or to
phenolphthalein (total acidity)
The difference between total acidity
and mineral acidity is actually
measure of free CO2
Chlorides
 When NaCl present in drinking water in conc of
250ppm or above give salty taste
 Cl- in high conc in H2O not toxic to human but
corrosive on pipes and harmful to plant life

Determination Mohar method

By using AgNO3 as titrant and K2CrO4
as indicator and E.P is red ppt
Fluoride in water
 F- occurs in some ground water
 Its limit in drinking water is mg/L to prevent dental
caries
 Excessive amount of F- cause an objectionable
discoloration of tooth enamel called fluorosis

Determination Colorimetrically by zirconium Alizarin

method
6F- +zirconium Alizarin(red) [ZrF]-+
free alizarin sulphonic from red to yellow
Water hardness and softing
 Hardness of water is caused principally by calcium and
magnesium and some times iron and aluminum
 Most of calcium and magnesium is resent in natural
waters as bicarbonates ,sulfates and sometimes
chlorides and nitrates
 Hardness producing substance s react with soap
forming insoluble compounds before lather is
produced
 They are measure of the soap destroying power of
water
Temporary hardness Permanent hardness
Caused mainly by presences of Caused mainly by Ca SO4 or presence of
bicarbonate salts of Ca2& Mg2 or due to Ca2+ & Mg2+ as SO42- ,Cl-&NO3- so called
Ca2+ & Mg2+ as CO32- and HCO3- so called non carbonate hardness
carbonate hardness

Removed by boiling (convert soluble Can not be removed by boling

bicarbonate to insoluble carbonate that Can be removed by ion exchange lime
removed by filtration soda process zeolite reverse osmosis

Acidic water contains non carbonate

hardness as Ca2+ & Mg2+ carbonate
caused water alkalinity
:

Determination of hardness
i. EDTA titration:
-Total hardness (Ca2+ + Mg2+): by titration using
eriochrome black-T indicator and ammonia buffer at pH 10.
- Calcium hardness: by titration using murexide indicator and
2N NaOH at pH 12.
- Magnesium hardness: = total - calcium hardness.
ii. Palmitate method (for total hardness):
Based on precipitation of calcium and magnesium palmitate,
at the end point, potassium palmitate (titrant) is hydrolysed to
give KOH (which changes ph. ph. colour).
iii. Soap method:
Depends on titration with soap solution (sodium oleate), end point is detected
by the formation of foam after precipitation of all Ca2+ and Mg2+.
iv. Soda reagent method:
Soda reagent is a mixture of equal volumes of 0.1N NaOH and 0.1N Na2CO3.
CaCl2 + Na2CO3  CaCO3 + 2 NaCl

MgCl2 + 2 NaOH  Mg(OH)2 + 2 NaCl

The excess reagent is measured after filtration by titration with N/50 sulphuric
acid using methyl orange indicator.
Permanent hardness (non-carbonate) consumes part of the alkalinity of soda
reagent .

- Temporary hardness does not consume alkalinity of soda reagent :

Ca(HCO3)2 + 2NaOH  2H2O + CaCO3 + Na2CO3
Mg(HCO3)2 + 4NaOH  2H2O + Mg(OH)2 + 2Na2CO3
2NaOH = H2SO4 and Na2CO3 = H2SO4
Total hardness is determined by neutralizing the sample firstly by N/50 H2SO4
(to MO), accordingly all CO32- and HCO3- are converted to SO42- and then
the solution is boiled to expel CO2. By soda reagent, it is not possible to
differentiate between Ca2+ and Mg2+.
Softening of water
 Removal of hardness from water by one of the
methods:
 - calcium and magnesium salts are precipitated from
water by chemical reagents crack method lime or soda
lim
 Substitution of Ca2+ & Mg2+ by Na+ as it don’t destroy
soap and not precipitating by heat so called non
hardness producing salts by passing hard water
through cation exchange zeolite
 The complete removal of all ions which causes
hardness “demineralization method”
Gases dissolved in water
 Hydrogen sulphide
 Oxygen dissolved
 H2s:
 It is poisonous ga s obtained from decomposition of
organic matter
 found in sewage & industrial waste water
 The toxicity of H2S is equivalent to that of HCN
Dissolved oxygen
 This means oxygen already dissolved or present in
water during its aeration
 Good water should have about 1 pm of dissolved
oxygen
 Bacteria is readily oxidized and destroyed by dissolved
oxygen
1. Winkler’s method: Oxygen oxidizes Mn2+ to Mn4+
which liberates iodine from KI/KOH, the liberated
iodine can then be titrated with thiosulphate:
 Mn2+ + 2OH-  Mn(OH)2
 Mn(OH)2 + ½ O2  MnO2 + 2H2O
 MnO2 + 2I- + 4H+  Mn2+ + I2 + 2H2O
 I2 + 2Na2S2O3  2NaI + Na2S4O6
Water pollution
Stages of purification of drinking water

1.Preliminary treatment: to remove large floating and

suspended solids. This is done by simple screening through a 5-
20 mm mesh screen.
2.Sedimentation: to remove smaller particles. This is done in
sedimentation tanks.
3.Coagulation and flocculation: to remove colloidal matters.
Coagulation (agglomeration of the colloidal particles) is the
reactions that take place upon the addition of a coagulant to water
. Flocculation (the process of building the coagulated particles).
The particles become large and dense enough to settle.
Coagulants (inorganic metal salts & organic polymers):

- Inorganic metal salts : Al2(SO4)3, Fe2(SO4)3, FeSO4,

FeCl3. Ferric salts act above pH 4.5 & ferrous salts act
above pH 9.5.
The most common coagulant is alum (aluminium sulphate):
Al2(SO4)3 + 6H2O  2Al(OH)3 + 3H2SO4
3H2SO4 + 3Ca(HCO3)2  3CaSO4 + 6H2CO3
6H2CO3  6CO2 + 6H2O

Al2(SO4)3 + 3Ca(HCO3)2  2Al(OH)3 + 3CaSO4 + 6CO2
- Organic polymers: Natural organic polymers (e.g. starch
and cellulose derivatives). Synthetic polymers (e.g.
polyethylene oxide polymers. These include cationic, anionic
and non-ionic polymers.
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Applications of coagulation:
Chemical Coagulation is used for removing of the
followings:
 Turbidity, organic and inorganic substances.
 Colour.
 Harmful bacteria and pathogens.
 Algae.
 Taste and odour-producing substances.
 Phosphates, which serve as nutrients for growth of
algae.

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Applications of coagulation:
Chemical Coagulation is used for removing of the
followings:
 Turbidity, organic and inorganic substances.
 Colour.
 Harmful bacteria and pathogens.
 Algae.
 Taste and odour-producing substances.
 Phosphates, which serve as nutrients for growth of
algae.

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4. Filtration: Achieved by flow through porous media,
usually sand. It is an important stage in the treatment
of potable water.
5. Disinfection: It is necessary to ensure the death
of harmful micro-organisms. This can be achieved by:

- Chlorine and its compounds.

- Ozone.
- Other disinfectants.
- Small scale disinfection
 I. Disinfection by chlorine and its compounds:
Advantages:
1. Readily available as a gas, liquid or powder.
2. Cheap.
3. Easy to apply due to its solubility (7 g/L).
4. It leaves a residual chlorine in solution, which provides
protection in the distribution system.
5. It is very toxic to most micro-organisms.
Disadvantages:
1. It is poisonous; requires careful handling.
2. Give rises to taste and odour problems (in presence of
phenols).
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Chemistry of chlorination:
Chlorine demand before disinfection: as chlorine is a
powerful oxidizing, it can combine with reducing agents
and unsaturated organic compounds:

H2S + 4Cl2 + 4H2O  H2SO4 + 8HCl

-CH=CH- + Cl2  Cl-CH-CH-Cl

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 Disinfection in absence of ammonia:
Cl2 + H2O HCl + HClO
Effective
H+ OH-
H+ + Cl- H+ + ClO-
(Free residuals) Ineffective
Disinfection in presence of ammonia:
Cl2 + NH3  NH2Cl + HCl
(monochloramine)
NH2Cl + Cl2  NHCl2 + HCl (dichloramine)
NHCl2 + Cl2  NCl3 + HCl
(trichloramine)
The combined residuals are more stable than the free residual
but less effective. Therefore, ammonia may be added to give
prolonged action.
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II. Disinfection by ozone: is a powerful oxidizing agent,
efficient disinfectant and much more expensive than
chlorination
III. Disinfection by other disinfectants: include heat,
ultraviolet/nuclear radiation, or bromine.
IV. Small scale disinfection (household-purification):
when pure water may not be obtainable, in emergency cases,
or during epidemic diseases.
- Boiling for 15 min., alum is added before boiling if water is
turbid.
- Chemical disinfection by very dilute KMnO4 solution.
- Using 2 drops of strong iodine solution (7 % per liter).
Using chloramine (3-4 mg/L) and allowed to stand for 30 min.
R-NH-Cl + H2O  RNH2 + HOCl
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