Dr. P.

Suresh Kumar

CHY101

Engineering Chemistry

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 Dr. P. Suresh Kumar

Course Objectives:

The main objectives of the course are to impart knowledge on the

fundamental chemistry principles involved in several important engineering
materials used in industry. In particular, the learners will study the basic
chemistry concepts and industrial applications of lubricants, redox reactions,
water treatment technologies and advanced engineering materials. The semi
theory – semi lab format of this course will also enable the learners to get
hands-on experience on the principles discussed during the theory classes
in the laboratory sessions where they will perform experiments to understand
the applications of these concepts in engineering.

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 Dr. P. Suresh Kumar

UNIT – I 11 Periods
WATER TREATMENT TECHNOLOGY

Definition of hard and soft water, Sources of water and classification of

impurities, Hardness and its types, Units of hardness, Determination of
hardness of water by EDTA method. Boiler problems – Scale and Sludge
formation in boiler, Priming & Foaming, Caustic Embrittlement. Internal
treatment methods. Water softening processes –Zeolite process, Ion-
exchange process. Brackish water treatment-Electrodialysis, Reverse
osmosis. BOD, COD- definition and significance. Sterilization - ozonolysis, UV,
chlorination, Specifications (Indian standards) for: Drinking water, Boiler feed
water, Water used in electronic and construction industries.

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UNIT – II 11 Periods
REDOX REACTIONS AND ELECTROCHEMISTRY

Electrochemistry - Single electrode potential, Nernst equation, Electrochemical

series and its applications. Electrolysis of water. Electrodeposition, Electroless
deposition, Plating on Plastics.

Energy devices -Primary battery (Alkaline battery), Secondary battery (Lead-

Acid, Ni-Cd and Li-ion). Supercapacitor- Principle. Fuel cells – Principle and
advantages, Hydrogen-Oxygen fuel cells, Proton exchange membrane fuel cell,
Alkaline fuel cell, Solid oxide fuel cell.

Corrosion and its control - Chemical and electrochemical corrosion, Microbial

induced concrete corrosion and biofouling. Corrosion control - Design, Anodic
and cathodic protection. Surface Coatings - Inorganic coatings (Galvanization,
Tinning, Electrode position, Anodization) and Organic coatings - oil paints.
Inhibitors (cathodic and anodic).
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 Dr. P. Suresh Kumar

UNIT –III 12 Periods

ASSOCIATIVE INTERACTIONS AND LUBRICANTS

Intermolecular interactions– ionic interactions, ion-dipole interactions,

hydrogen bonding, dipole-dipole interactions, London dispersion forces.
Relative strength of intermolecular forces - H2O-H2S, HCl-HF, Ethanol-diethyl
ether, Polyethylene-Teflon. Consequences - surface tension.

Lubricants- Mechanisms of lubrication - Fluid film, Boundary film & Extreme

pressure. Types of lubricants – Solid lubricants – Molybdenum disulphide,
Graphite. Liquid lubricants – Vegetable, Animal, Mineral & Synthetic oils. Semi
solid lubricants – Greases, Lubricating Emulsions – Oil in water, Water in oil.
Properties of lubricants and its significance – Physical properties – Viscosity
& Viscosity Index. Determination of viscosity by Redwood viscometer, Flash &
Fire point by Pensky- Marten’s apparatus, Cloud & Pour point. Lubricating oils
– Acid value, Saponification value, Steam emulsification number.

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 Dr. P. Suresh Kumar

UNIT – IV 11 Periods
ADVANCED MATERIALS

Composites –Introduction, Constitution-Matrix phase, Dispersed phase.

Characteristic properties of composite materials. Classification- (A) Particle -
reinforced composites- i) Large – particle reinforced composites ii) Dispersion
– strengthened composites. (B) Fiber – reinforced composites- i) Continuous –
aligned ii) Discontinuous – aligned (short)- (a) aligned (b) randomly oriented
(C) Structural Composites- i) Laminates (ii) Sandwich Panels.

Nanomaterials-Classification. Synthesis–Top down method (Ball milling),

Bottom up methods – wet chemical, physical and chemical vapor deposition,
Sol-Gel method, Self- assembly (DNA-directed self-assembly of AuNPs),
Applications of nanomaterials – AuNPs based anti-cancer agents, ZnO and
Fe3O4 based memristors, Water purification using AgNPs, TiO2 based self-
cleaning glass.

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 Dr. P. Suresh Kumar

Why Engineering Chemistry?

Role of chemistry in our life- irrespective of the branch you

have chosen!!

Demand for good quality water- fundamental right!

Availability of quality water resources- hard water, fluoride,

microbes,..

Treatment of waste water- treatment methods - chemical

methods

Evaluation of water quality

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Electrochemistry

Oxidation/reduction reactions

At equilibrium conditions- reduction potential values- Nernst

equation- electrode potential – applications – deposition of metals

Energy storage devices – batteries, supercapacitors, fuel cells

Corrosion - Reason, mechanism, how to avoid

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Intermolecular interactions

Type of interactions

Structure formation

Atoms- molecules- supramolecules- proteins, enzymes-

organs- living species

Interactions around our surroundings

Properties of molecules/ materials

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Lubricants

Associative interactions should be minimal to reduce friction

Role of lubricants

Chemistry of lubricants

Types of lubricants

Physical/chemical properties of lubricants

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Advanced materials

Why to look into material science/material chemistry?

Individual materials to composite materials

Types of composites

Properties of composites

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Advanced materials - Nanomaterials

Nanomaterials - importance/ significance

Synthetic methods

Applications

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Unit 1: Water treatment Technology

Water (H2O) – One of the most essential molecule for life!!

For humans-> Domestic/agriculture/ industry/ ...

Availability of water on earth - ~ 97 % in ocean as saline water

Available directly as pure water ~ 1 %

(~ 2 % in glaciers, ice caps, rock crevices,...)

Water is very valuable !!!!

Treat the water: waste water/ocean water/other resourses

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Water resources
●
Surface water – water streams, rivers, ponds, lakes,...
●
Underground water- springs/wells/coal mines
●
Sea water
●
Rain water

Hardness of water
Presence of dissolved minerals hardness & alkalinity

What is hardwater?
Soap consuming capacity
Soap/detergents: Na/K salts of higher fatty acids
Precipitation of soap in hardwater

2C17 H 35 COONa+CaCl2 →(C 17 H 35 COO)2 Ca↓+2NaCl

Sodium stearate Calcium soap
Insoluble salt

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Hardness of water:
Presence of soluble salts of Ca2+, Mg2+, Fe3+, Al3+, Mn2+
Soap will be precipitated!!!
Most prominent ions causing hardness: Ca2+ and Mg2+
Other ions may be in trace amount

Any cation which forms insoluble salt with soap contributes to hardness

What about anions?

Dissolved CO2 in water – carbonic acid- precipitate soap as fatty acid
For practical purposes, only cations are considered!!!

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Temporary and permanent hardness

Boiling the water containing Ca or Mg bicarbonate

Decomposition & precipitation of carbonate salt

Ca(HCO 3)2 →CaCO 3 ↓+H 2 O+CO 2

Mg(HCO3 )2 → MgCO 3 ↓+H 2 O+CO 2

Insoluble in water

Elimination of hardness => temporary hardness

Boiling of CaCl2 etc will not lead to insoluble salts => permanent hardness

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Temporary hardness : carbonate hardness (alkaline hardness)

hardness due to dissolved bicarbonates, carbonates, hydroxides
=> Can be estimated by titrated against mineral acid using methyl
orange indicator

Permanent hardness: non-carbonate hardness (non-alkaline hardness)

Hardness due to dissolved chlorides, sulphates, nitrates mostly of Ca2+ or Mg2+

Total hardness = Temporary hardness + Permanent hardness

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Representation (Unit) of hardness

Quantification of hardness (amount of salts causing hardness)

Mostly Ca2+ and Mg2+ ions
Represented as equivalent weight of a single salt
Calcium carbonate (CaCO3) with molecular weight of 100 as a convenient one
Typical values are several 100s of mg per L of water

1 L water = 1 kg of water 106 = 1 million

mg of salt / kg of water = mg salt/ 106 mg water
==> 1 part /106 part ==> parts per million (ppm)

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1 ppm = 1 mg/L of CaCO3 equivalent

100 mg CaCO3 =

111 mg CaCl2 95 mg MgCl2

136 mg CaSO4 120 mg MgSO4 Atomic weight of Ca: 40.078

162 mg Ca(HCO3)2 146 mg Mg(HCO3)2 Atomic weight of Mg: 24.305
164 mg Ca(NO3)2 44 mg of CO2

For example:
81 mg/L of Ca(HCO3)2 = 81*100/162 = 50 mg/L = 50 ppm

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Example1: Calculate the temporary and permanent hardness of a sample of

water containing the following impurities: Mg(HCO3)2: 73 mg/L; Ca(HCO3)2: 162
mg/L; CaSO4: 136 mg/L; MgCl2: 95 mg/L; CaCl2: 111 mg/L; NaCl: 100 mg/L
NaCl does not contribute to hardness!!!
Solution:
Convert all of them in terms of CaCO3 eq (molar wt 100)

Temporary hardness: Mg(HCO3)2 and Ca(HCO3)2 with molar weight 146 and 162
respectively
73∗100 162∗100
Temporary hardness = + =50+100=150 mg/ L=150 ppm
146 162
Permanent hardness: CaSO4, MgCl2 and CaCl2 [molar wt 136, 95 and 111
respectively]
136∗100 95∗100 111∗100
Hence permanent hardness = + + =100+100+100=300mg/ L=300 ppm
136 95 111
Total hardness = 150 + 300 = 450 ppm

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Example2: Calculate the temporary and permanent hardness of a sample of

water whose analysis is as follows: Mg(HCO3)2: 50 mg/L; Ca(HCO3)2: 40 mg/L;
CaSO4: 48 mg/L; MgSO4: 35 mg/L; NaCl: 20 mg/L

Solution: No contribution from NaCl towards hardness

Convert all of them in terms of CaCO3 eq (molar wt 100)

Temporary hardness: Mg(HCO3)2 and Ca(HCO3)2 with molar weight 146 and 162
respectively
50∗100 40∗100
Temporary hardness = + =34.25+24.69=58.94 mg/ L=58.94 ppm
146 162
Permanent hardness: CaSO4 and MgSO4 [molar wt 136 and 120 respectively]
48∗100 35∗100
Hence permanent hardness = + =35.29+29.17=64.46 mg / L=64.46 ppm
136 120
Total hardness = (58.94 + 64.46) ppm = 123.4 ppm

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Example 3: Calculate the temporary and permanent hardness of a sample that

contains the following impurities: Ca(HCO3)2: 12.5 ppm, Mg(HCO3)2: 120 ppm;

MgCl2: 80 ppm, CaSO4: 130 ppm and Ca(NO3)2: 30 ppm

Solution:

Temporary hardness (due to Ca(HCO3)2 and Mg(HCO3)2 )

= 12.5*100/162 + 120*100/146 = ...........ppm

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Determination of hardness – EDTA method

Complexometric titration

EDTA: Ethylenediaminetetraacetic acid

Disodium salt of EDTA: Na2H2Y

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Tetra or hexa dentate ligand for metal binding

M-EDTA complex (colorless)

Eriochrome Black- T (EBT) as indicator

EDTA

M-EDTA

M + EDTA → M −EDTA
EBT M-EBT All colorless

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Principle of hardness estimation:

Hard water + ammonia buffer + EBT indicator
Ca2+/Mg2+ NH4Cl / NH4OH (pH 9-10)

M +EBT → M −EBT
colorless steel blue wine-red

Titration against EDTA:

M−EBT +EDTA → M−EDTA +EBT

wine-red colorless colorless steel blue

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Procedure for hardness estimation by EDTA method

Titration 1: Standard hard water (20 mL) vs EDTA

Std hard water: 1000 mg/L of CaCO3 eq. (1000 ppm)

1 mL of standard hard water = 1 mg of CaCO3 equivalent

V1 mL of EDTA = 20 mg of CaCO3 equivalent

1 mL of EDTA = 20/ V1 mg of CaCO3 equivalent

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Titration 2: standardised EDTA vs sample hard water (V3 = 40 mL)

V3 mL of sample hard water = V2 mL of EDTA

= V2 x 20/ V1 mg of CaCO3 equivalent

1000 mL of sample hard water = (1000/V3) x V2 x (20/ V1) mg of CaCO3 eq.

= ..........mg of CaCO3 eq.

Total hardness = ....... mg of CaCO3 equivalent

....... ppm of CaCO3 equivalent

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Example: 0.5 g of CaCO3 was dissolved in dil HCl and diluted to 500 mL. 50 mL
of this solution required 48.0 mL of EDTA solution for titration. 50 mL of a hard
water sample required 15 mL of EDTA solution for titration. 50 mL of same
hardwater on boiling, filtering etc required 10 mL of EDTA solution. Calculate
different kinds of hardness.
Solution: 15∗50 1000
500 mL std hard water = 0.5 g CaCO3 = 500 mg CaCO3 total= ∗
48.0 50
1 mL std hard water = 1 mg CaCO3 eq
48.0 mL EDTA = 50 mL std hardwater 10∗50 1000
permanent= ∗
1 mL EDTA = 50/48.0 mg of CaCO3 eq 48.0 50
50 mL sample water = 15 mL EDTA = 15 * 50/48.0 mg CaCO3
1 L sample water = 15 * 50/48.0 * 1000/50 = 312.5 mg CaCO3 = 312.5 ppm
(total hardness)
50 mL boiled water = 10 mL EDTA = 10*50/48.0 mg CaCO3 eq
1 L of boiled water = 10*50/48.0 * 1000/50 = 208.3 ppm (permanent hardness)
Temporary hardness = 312.5 – 208.3 = 104.2 ppm
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Alternative solution:
M1V1 = M2V2
100 g CaCO3 in 1 L water = 1 M ==> 1 g CaCO3 / L => 0.01 M

0.5 g CaCO3 in 500 mL water = 0.01 M

Titration 1: Vstd x Mstd = VEDTAx MEDTA => 50x 0.01 = 48 x MEDTA

==> MEDTA = 0.010417 M

Titration 2 : sample water before boiling (total hardness)
VEDTAx MEDTA = Vsamplex Msample ==> 15 x 0.0104 = 50 x Msample ==> Msample = 0.003125 M
==> 0.003125 x 100 g => 0.3125 g ==> 312.5 mg/L = 312.5 ppm
After boiling: (permanent hardness)
VEDTAx MEDTA = Vsamplex Msample ==> 10 x 0.0104 = 50 x Msample ==> Msample = 0.002083 M
==> 0.002083 x 100 g => 0.2083 g ==> 208.3 mg/L = 208.3 ppm
Temporary hardness = total – permanent = 312.5-208.3 = 104.2 ppm
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Example: Calculate hardness of a water sample whose 100 mL required 20

mL EDTA. 20 mL of CaCl2 solution whose strength is equivalent to 1.05 g of

CaCO3 per liter required 30 mL EDTA.

Solution:
1 L std hard water = 1.05 g CaCO3 eq/L

1 mL std water = 1.05 mg CaCO3 eq

20 mL std water = 30 mL EDTA
1 mL EDTA = 20/30*1.05 mg CaCO3 eq

100 mL sample water = 20 mL EDTA = 20*20/30 * 1.05 CaCO3 eq = 14 mg

CaCO3 eq
1 L sample water = 14*10 mg = 140 ppm
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Example: 250 mL of water is boiled for half an hour and filtered. The filtrate
is made up to 250 mL with distilled water. 50 mL of this water required 4 mL
of 0.02 M EDTA solution with an NH4OH-NH4Cl buffer and EBT indicator.
Calculate permanent hardness of the sample.
Solution:
Vsample * Ssample = VEDTA * SEDTA

Ssample = VEDTA * SEDTA /Vsample = 4*0.02/50 = 1.6x10-3 M

= 1.6x10-3 * 100 g/L = 160 mg/L = 160 ppm

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Example: 0.01 g of CaCO3 dissolved in water to which HCl was added required
22 mL of EDTA. 100 mL of hard water required 26 mL of EDTA. 100 mL of the
same sample of water after boiling and filtering required 18 mL of EDTA. Find
out the carbonate and non-carbonate hardness of water.
Solution:
22 mL EDTA = 0.01 g CaCO3 eq = 10 mg

1 mL EDTA = 10/22 mg CaCO3 eq

100 mL hard water = 26 mL EDTA
1L hard water = 10*26 mL EDTA = 10*26*10/22 mg CaCO3 eq

= 118.18 mg CaCO3 eq = 118.18 ppm (total hardness)

Continued...

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100 mL boiled water = 18 mL EDTA

1 L boiled water = 10*18*10/22 mg CaCO3 eq = 81.8 ppm
Non carbonate hardness = Permanent hardness = 81.8 ppm
Carbonate hardness = temporary hardness = 118.18-81.8 = 36.38 ppm

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Disadvantages of hardness:
a) washing and bathing
b) Drinking and cooking
c) Industrial purpose
●
textile industry
●
paper industry
●
sugar industry
●
dying industry
●
boilers

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Disadvantages of hardness:

a) washing and bathing

Lack of leathering of soap - sticky Ca or Mg soap precipitate
After complete precipitation of Ca or Mg, leather formation- wastage of soap !
Sticking of precipitate on cloth => spot formation
Iron in trace amount => stain formation (colored iron soap)
Drying of skin during bathing – may cause allergy

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Disadvantages of hardness:

b) Drinking and cooking:

Damage in digestive system
Formation of calcium stone in urinary tract and/or bladder
Elevation in boiling point – more energy to boil water
Cooked pulses may not be soft
Taste difference
Precipitation of CaCO3 in inner walls of container reduced heat transfer
(boiler problems)

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Disadvantages of hardness:
c) Industrial purpose
●
boiler issues
●
Textile industry: soap wastage, precipitate on fabric- interference in later
steps, color fading
●
Paper industry: Interference of Ca2+ and/or Mg2+ with chemicals
Loss of quality of paper- loss of glossiness, smoothness, color
●
Sugar industry: difficulty in crystallisation and storing
●
Dying industry: Reaction of hardness causing ions with functional groups
of dye => precipitation or alteration of shades

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Boiler problems
Boilers: For steam generation in industries/ power houses

If hard water is supplied to boiler:

●
Scale and sludge formation
●
Priming and foaming
●
Caustic embrittlement
●
Boiler corrosion

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Scale and sludge formation

In boilers, water is continuously evaporates => concentration of salts increases

Solubility product & saturated solution
Precipitation of solutes/salts on inner walls
If soft, loose & slimy ==> sludge
If hard & adhering => scale

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Scale and sludge formation

Sludge formation: Due to MgSO4, MgCl2, MgCO3 and CaCl2

●
High solubility in hot water than cold water
●
Sludge formation at colder parts of boilers &
Get collected at places where flow rate is less
●
Can be easily removed by blow-down operation
●
Poor conductors of heat- choking of pipe
●
Prevented by softened water

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Scale and sludge formation

Scale formation
●
Firmly sticking hard substances
●
Can not be removed by mechanical abrasion
●
Major couse of boiler problems !!
●
Formation:
1) Decomposition of calcium bicarbonate Ca(HCO 3)2 →CaCO 3 ↓+H 2 O+CO 2
2) low solubility of CaSO4 at high temperature- precipitate as hard
scale at hotter parts of boiler – mostly in high pressure boilers !!
3) Dissolved Mg salts on hydrolysis at high T - MgCl 2 +H 2 O→ Mg(OH)2 +2 HCl↑
4) Conversion of trace SiO2 to CaSiO3, MgSiO3- too difficult to remove

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Scale and sludge formation

Problems with scale formation

●
Poor thermal conductors-acts as heat insulators – high energy
consumption
Depends on the thickness
●
Need to be overheated to maintain steady supply of steam
●
Decrease efficiency of boiler
●
If crack forms in scale, water in contact with overheated boiler- sudden
increase in steam- boiler explosion

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Scale and sludge formation

Removal of scale formation
# Mechanical methods to remove scales

by thermal shocks

Loosely sticking scale removal by scrapping
# Chemical methods
 Removal of basic scales (such as CaCO3): dissollution by 5-10 % HCl
solution
 CaSO4 & silicate scale removal by dissolving with EDTA – high solubility
of EDTA complex
Prevention:

Treatment of boiler feed water
➔
Internal and external treatment methods
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Priming and foaming in boiler

Priming:
●
When steam produced rapidly, water droplets with steam (wet steam)
Why?
●
Large amount of dissolved salts, sudden boiling, high steam velocity,
Improper design
How to avoid:

Efficient softening of boiler feed water

Controlling rapid change in steam velocities

Mechanical steam purifiers

Proper design of boiler (with low water levels)

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Priming and foaming in boiler

Foaming:
Formation of foam in boiler that do not break easily
Major contribution: oily particles-decrease surface tension of water
Mostly occur together with priming !!
Carried over of dissolved salts – deposit in turbine blades & machinary parts
===> Damage to machine parts
Prevention of foaming
Addition of NaAlO2 to remove oily particles from water
Addition of anti-foaming agents – eg: castor oil

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Caustic embrittlement:
●
A type of boiler corrosion by highly alkaline water in high pressure boilers
● High amount of residual Na2CO3 in water (due to Lime-soda process)
Na2 CO 3 +H 2 O→2 NaOH +CO 2 ↑
●
NaOH => more alkaline water (or caustic) => move to small cracks in boiler
●
With evaporation of water, concentration increases
●
Attack on iron of boiler ==> sodium ferrate
=>Embrittlement, boiler walls become weak => boiler damage
●
More damage to high stress parts - riverts, joints & bends

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Caustic embrittlement:

Concentration cell formation:

Anode: con. NaOH & cathode: dil. NaOH

Prevention:
●
Adjustment of boiler feed water pH between 8-9
● Use of sodium phosphate instead of Na2CO3 during external treatment
● Addition of tannin or Na2SO4 => blocks the hairline cracks

Preventing the infiltration of Na2CO3 to the cracks

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Boiler corrosion

Disintegration of body of boiler due to chemical/electrochemical reaction

Major contributors:

● Acids due to hydrolysis of dissolved salts (eg MgCl2)

● Dissolved CO2

● Dissolved O2

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Boiler corrosion
Hydrolysis of salts:
MgCl 2 +2 H 2 O→ Mg(OH)2 ↓+2HCl

Fe+2 HCl →FeCl 2 +H 2 ↑

FeCl2 +2 H 2 O→ Fe(OH )2 ↓+2 HCl

4 Fe(OH )2+O2 → Fe 2 O 3 .3 H 2 O
rust
Regeneration !!! => cyclic reaction of HCl => extensive damage

Even small amount of MgCl2 is dangerous !!!

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Boiler corrosion
Dissolved CO2 => formation of carbonic acid
CO 2+ H 2 O→ H 2 CO 3
=> corrosion under acidic condition

Source of CO2: dissolved bicarbonates

Ca(HCO 3)2 →CaCO 3 ↓+H 2 O+CO 2

How to avoid:
●
Mechanical deaeration
● Addition of NH4OH
2 NH 4 OH+CO 2 →( NH 4 )2 CO 3 +H 2 O

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Boiler corrosion
Dissolved oxygen => at room temperature ~ 8 ppm
Corrosion of boiler at high temperature

2 Fe+2 H 2 O+O2 →2Fe (OH)2↓

4 Fe(OH )2+O2 → Fe 2 O 3 . xH 2 O rust
How to avoid?
Addition of hydrazine, sodium sulphite or sodium sulphide or
mechanical deaeration
N 2 H 4 +O2 → N 2+2 H 2 O 2 Na2 SO3 +O2 → 2 Na2 SO4 Na2 S+2O2 → Na2 SO 4
Hydrazine is ideal reagent !!
Na2SO4 decompose to form SO2 at high pressure => H2SO3 => corrosion !!

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Treatment of water

External treatment
●
Zeolite process
●
Ion exchange process

Internal treatment
●
Carbonate conditioning
●
Colloidal conditioning
●
Sodium aluminate
●
Phosphate conditioning
●
Calgon conditioning
●
Electrical conditioning

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Zeolite (permutite) process

Natural or synthetic minerals; zeolite = boiling stone

Common formula for sodium zeolite: Na2O.Al2O3. XSiO2. Y H2O X : 2-10; Y: 2-6
Hydrates sodium aluminosilicates
Can reversibily exchange 2 Na+ ions with alkaline earth metal cations
Natural zeolite: amorphous, obtained from green sands by washing, heating &
treat with NaOH
Eg: natrolite Na2Al2O3. 4SiO2. 2H2O
Synthetic zeolite: porous; heating sodium silicate + aluminium sulphate +
sodium aluminate
Better exchange capacity than natural zeolite / unit weight

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Zeolite (permutite) process - Principle

Na2O.Al2O3. XSiO2. Y H2O ===> represented as Na2Z => sodium zeolite
Passage of hard water through zeolite
=> exchange of cations => Ca or Mg zeolite

CaCl2 +Na2 Z →CaZ +2 NaCl MgCl 2 +Na2 Z→ MgZ+2NaCl

CaSO 4 +Na2 Z→CaZ +Na2 SO 4 MgSO4 +Na2 Z → MgZ+Na 2 SO4

Ca(HCO 3)2 +Na2 Z →CaZ +2 NaHCO 3 Mg(HCO3 )2 +Na2 Z → MgZ+2NaHCO 3

Exhausted zeolite: Regeneration

CaZ+2NaCl →CaCl2 +Na2 Z MgZ+2 NaCl→ MgCl 2+Na 2 Z

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Zeolite (permutite) process – Procedure

Regeneration using ~ 10 % NaCl solution

Residual hardness: 0-15 ppm

Presence of Na+ salts

Precausion:
●
Turbidity : clogging of pores
●
Fe2+, Mn2+ ions: irreversible FeZ, MnZ
●
Mineral acid: zeolite degradation

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Ion exchange process:

Removal of all cations and anions ==> demineralisation or deionisation !!

Use of resins ==> organic, cross-linked insoluble polymer with functional groups
Cation exchange resin (cation exchangers) :
Contain acidic functional group: -COOH or -SO3H
Can exchange proton (H+) with cations
Anion exchange resin (anion exchangers) :
Contain basic functional groups: -NH2, =NH, etc
As hydroxides or hydrochlorides==> Can exchange anions
Based on extent of acidity and/or alkanity,
==> strongly acidic, weakly acidic
==> strongly basic, weakly basic
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Cation exchange resin:

Styrene-divinyl benzene copolymers
sulphonation or carboxylation ==> proton exchange capacity
R-H+ => R-: resin part
Examples: Amberlite IR-120, Dowex-50

R- H + +Ca2+ → R2 Ca+2 H +

R- H ++Mg 2+ →R 2 Mg+2H +

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Anion exchange resin:

Styrene-divinyl benzene or Amine-formaldehyde copolymers
Amino or quarternary ammonium groups ==>
Treatment with dil NaOH ==> hydroxide (OH-) exchange capacity
R+OH- => R+: resin part
Examples: Amberlite 400, Dowex-3

+ - -
R OH +Cl → RCl+OH - 2 R+ OH - +SO2-4 →R 2 SO4 +2OH -

+ - 2-
2 R OH +CO →R 2 CO 3 +2OH
3
- R+ OH - + HCO-3 → RHCO3 +OH -

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Cation exchange reactions Anion exchange reactions

CaCl2 +2 R−H → R 2 Ca+2 HCl

MgCl 2 +2 R−H → R2 Mg+2 HCl

CaSO 4 +2 R−H → R 2 Ca+H 2 SO4 R+ OH - +Cl - → RCl+OH -
+ - 2- -
MgSO4 +2 R−H → R2 Mg+ H 2 SO4 2 R OH +SO →R 2 SO4 +2OH
4
+ - 2- -
2 R OH +CO →R 2 CO 3 +2OH
Ca(HCO 3)2 +2 R−H → R 2 Ca+H 2 CO 3 3
+ - - -
Mg(HCO3 )2 +2 R−H → R 2 Mg+H 2 CO 3 R OH + HCO → RHCO3 +OH
3

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 Dr. P. Suresh Kumar

Schematic representation of ion exchange plant:

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 Dr. P. Suresh Kumar

Exhausted resin:

Regeneration of cation exchange resin

=> treatment with acid (dil. HCl or dil. H2SO4)

R2 Ca+2 H + →2RH +Ca2+

Regeneration of anion exchange resin
=> treatment with dil. NaOH R2 SO 4 +2OH - →2 ROH +SO2-4

Residual hardness: 0-2 ppm

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 Dr. P. Suresh Kumar

Internal treatment methods:

Only as supplimentary to external treatment !!
i) Carbonate conditioning
For low pressure boilers
Removal of CaSO4 and other scale forming salts by addition of Na2CO3

CaSO 4 +Na2 CO 3 →CaCO3 ↓+Na2 SO4

ii) Colloidal conditioning
Addition of tannin, agar agar or kerosene
Adsorption over scale forming solid
==> prevents aggregation to hard deposits
==> loose deposits removal by blow-down operation

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 Dr. P. Suresh Kumar

Internal treatment methods:

iii) Treatment with sodium aluminate
Hydrolysis: NaAlO 2 +2 H 2 O→ NaOH + Al(OH )3 ↓

Reaction with Mg salts and its precipitation

MgCl2 +2 NaOH → Mg(OH)2↓+2 NaCl

Al(OH)3 and Mg(OH)2 as flocculant precipitate
==> absorb on suspended colloidal particles (silica, oil, ..) and precipitates

Removal of the loose precipitates by blow-down operation

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 Dr. P. Suresh Kumar

Internal treatment methods:

iv) Phosphate conditioning
Suitable for high pressure boilers as well
Addition of NaH2PO4, Na2HPO4 or Na3PO4 (depends on pH of solution)
Optimum pH : 9.5 to 10.5
If feed water is highly alkaline : NaH2PO4

If feed water is highly acidic : Na3PO4

Reaction with Ca/Mg salts ==> soft sludge of Ca/Mg phosphate
=> blow-down operation

3CaCl2 +2Na3 PO 4 →Ca3 ( PO 4 )2 ↓+6 NaCl

3 MgCl 2 +2 Na3 PO 4 → Mg 3 (PO 4 )2 ↓+6 NaCl
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 Dr. P. Suresh Kumar

Internal treatment methods:

v) Calgon conditioning (NaPO 3)6
Calgon: sodium hexametaphosphate ==> popular choice for treatment
Conversion of highly soluble hardness causing metal ions to soluble
complexes

Na2 [ Na4 (PO 3 )6 ] ⇌ 2 Na+ +[ Na4 P6 O18 ]2-

2CaSO 4 +Na2 [ Na4 P6 O18 ] ⇌ Na2 [Ca 2 P6 O18 ]+2Na2 SO 4

Soluble complex

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 Dr. P. Suresh Kumar

Internal treatment methods:

vi) Electrical conditioning

Sealed glass bulbs filled with mercury => connect with battery

==> Electrical discharges by mercury bulb

Prevention of coalescence of scale forming solids

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 Dr. P. Suresh Kumar

Quality of drinking water

What is expected?

WHO: World Health Organization

ISI: Indian Standards Institution
USPH: United States Public Health Service

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Dr. P. Suresh Kumar

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 Dr. P. Suresh Kumar

Treatment methods for drinking water

Per day: adult male : ~ 2.9 L; adult female: ~ 2.2 L, children: ~ 1.0 L
Availability of drinking water?
Contaminants and its removal ==> treatment methods

●
Screening
●
Sedimentation
●
Sedimentation with coagulation
●
Filtration
●
Disinfection

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 Dr. P. Suresh Kumar

Screening:

The raw water passed through screens having larger number of holes
Holds back floating matters (wood pieces, leaves, larger and heavier objects..)

Aeration and sedimentation:

Allowing for aeration in big tanks to exchange of gases between water and air
==> amplifies the oxygen content
==> removal of iron, manganese and dissolved gases like H2S, CO2 and NH3
==> gravitational force
=> high density suspended particles settle down at bo

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 Dr. P. Suresh Kumar

Sedimentation with coagulation:

Simple sedimentation does not remove the finely divided silica, clay &
organic matter
Addition of coagulants (alum, sodium aluminates and aluminium sulphate)
==> gelatinous precipitates (flock)
Flock attracts and facilitates the accumulation of the colloidal particles,
==> settling of the colloidal particles
==> Flocculation

Al2 (SO4 )3 +3Ca(HCO 3)2 →2 Al(OH )3 ↓+3CaSO 4 +6CO 2 ↑

Addition of Na2CO3 if natural alkalinity is not present

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 Dr. P. Suresh Kumar

If pH range is 5.5 to 8.5, NaAlO2 is ideal

NaAlO 2 +2 H 2 O→ Al(OH)3 ↓+NaOH

Flocculent ppt

MgCl 2 +2 NaOH → Mg(OH) 2↓+2 NaCl

Advantanges of NaAlO2 coagulant:
=> To remove finely divided particles
=> To reduce Mg hardness

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 Dr. P. Suresh Kumar

Filtration:

For removing micro-organism, color and odour

Different variations Fine sand

●
Gravity filter
Coarse sand
●
Slow sand filter
Large grannular
●
Rapid sand filter material
●
Pressure filter

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 Dr. P. Suresh Kumar

Disinfection
Disruption of harmful microorganisms
Through disinfection, complete removal of microorganism not possible
==> sterilisation by boiling the water

Ideal disinfectant: should remove all pathogens

●
Quickly
●
At room temperature
●
Inexpensive
●
Should not be toxic to humans
●
Should provide protection against contamination during
conveyance or storage

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 Dr. P. Suresh Kumar

Disinfection
Chlorine as disinfectant
●
Chlorine gas passing through water
●
Aquous solution of chlorine gas (dissolved in water) is added to
water sample
●
Added as bleaching powder
Optimal amount for effective disinfection
When added as bleaching powder:
Ca(OCl)2 +H 2 O→Ca(OH)2 + HOCl Ca(OCl)2 +HCl→Ca(OH)2 +Cl 2
Cl 2+ H 2 O→ HCl +HOCl Hypochlorous
H acid, unstable
y
p
HOCl→ HCl+[O] Nascent oxygen

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 Dr. P. Suresh Kumar

Disinfection
Nascent oxygen distroys pathogens by oxidation
OCl- rupture cell membrane
Cl2 has antimicrobial activity

Drawback of bleaching powder:

●
Unstable during storage
● Introduces Ca hardness ==> Cl2 is preferred

Excess usage of Cl2 or bleaching powder

==> pungent odor, bad taste, irritation to mucous membranes
=> Can overcome by addition of NH3 ==> formation of NH2Cl

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 Dr. P. Suresh Kumar

Breakpoint chlorination

Step 1: Added chlorine is consumed to oxidize easily oxidisable chemicals

eg: H2S, Fe2+, Mn2+, ...
Step 2: Added chlorine reacts with organic matter including microorganism
==> formation of chloroorganic compounds without degradation
If NH3 is present ==> formation of chloramines
Step 3: Oxidation of organic compounds generated from microorganisms
Cl2 is consumed, residual Chlorine reaches a minimum when
oxidation is complete ==> break point chlorination
Step 4: Applied chlorine is not used for any reaction

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 Dr. P. Suresh Kumar

Destruction Free chlorine

Formation of
Oxidation of formed
chlroroorganics organic
of and chloramines
reducing compounds
Residual chloride

species

1 2 3 4

Applied Chlorine
Drawback: Generation of harmful chloroorganic compounds
Trihalomethanes, haloacetic acid (carcinogenic)
==> need to reduce organic part before chlorination

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 Dr. P. Suresh Kumar

Ozonation
Strong, broad spectrum disinfectant against almost all microorganisms
Highly unstable, readily absorbed by water and breaks down to give
nascent oxygen
O3 →O2 +[O]

Nascent oxygen => powerful oxidizing agent

==> kills bacteria & oxidation of organic matter
O3 is unstable ==> in situ production !! ==>expensive & not in large quantity

When Br content is more ==> formation of carcinogenic bromate !!

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 Dr. P. Suresh Kumar

Ultraviolet treatment:
UV light as efficient method to inactivate dangerous protozoans that form cysts

Works effectively against almost all microorganisms

Widely used as disinfectant in swimming pool water

Potassium permanganate (KMnO4)

=> another disinfectant used in well water

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 Dr. P. Suresh Kumar

Desalination
Removal of common salts (mostly sodium chloride, NaCl) from the water
Brackish water and sea water ==> to potable water
Quality:
Fresh water: < 0.05% of dissolved solids
Brackish water: > 0.05% < 3.5% of dissolved solids
Sea water: > 3.5% of dissolved solids
Brine water: Contains > 5% of dissolved solids with maximum of 26-28 %

Methods:
●
Electrodialysis
●
Reverse osmosis

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Electrodialysis

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Reverse osmosis

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 Dr. P. Suresh Kumar

Treatment of sewage water

Sewage or waste water: water coming from general cleaning, washing
cloths, bathing and flushing the toilet

Common parameters:
●
Biological oxygen demand (BOD)
●
Chemical oxygen demand (COD)
●
Total suspended solids (TSS)
●
pH
●
Total phosphor

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 Dr. P. Suresh Kumar

Biological oxygen demand:

Amount of dissolved oxygen that would be consumed if all organics in one liter
of water were oxidized by protozoa and bacteria

High BOD ==> excess amounts of organic pollutant => high polluting power !!

Domestic sewage 200-600 mg/L

Vegetable processing 200-5,000 mg/L
Slaughterhouse waste 1,000-4,000 mg/L
Cattle shed effluents > 20,000 mg/L

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 Dr. P. Suresh Kumar

Chemical oxygen demand:

Amount of dissolved oxygen that would be consumed if all organics in
one liter of water were oxidized by potassium dichromate
Accepted range: < 10 ppm

pH: Concentrations of hydrogen ions in water ==> level of acidity or

alkalinity
Normal range: 5-10
Abnornal pH => interfere with biological process

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 Dr. P. Suresh Kumar

TSS: Sum of the concentrations of inorganic and organic solids

Suspended solids: Solids present as suspension with water
=> 30% inorganic + 70% organic solids
Elimination by physical or mechanical methods

Organic solids: Urban waste water => 50 % of solids from the waste products of
vegetable and animal life ==> Volatile solids or combustible fractions => removal
at high temperature

Inorganic solids: Inert substances ==> mud, sand and gravel => will not decayed

Settleable solids: Subset of suspended solids => suspended solid fraction =>
settle over time

Colloidal suspended solids: colloidal dispersion => Not a solution/ will not settle
readily
(may be organic and/or inorganic particles)

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 Dr. P. Suresh Kumar

Water specification for different sectors

Healthcare:

Patients susceptible to infectious agents (bacteria, virus,..)

Drink boiled water
Injection solutions: highest level of chemical purity, completely sterile (free
from pathogens)
Injection grade by distillation and/or high pressure reverse process
For washing during surgical procedure & for cleaning surgical tools

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 Dr. P. Suresh Kumar

Water specification for different sectors

Electronic industry: Ultrapure water for semi-conductors and printed circuit

board
Contain only H2O
Residual mineral limit: in parts per trillion (ppt: 1 in 1012) levels
total organic carbon (TOC): ppb (parts per billion, 1 in 109) level
Conductivity : 0.055 μS/cm at 25 oC (Resistivity of 18.2 MΩ.cm)
Preparation: gross filtration, carbon filtration, chemical dosing for
softening, reverse osmosis, exposure to ultraviolet to control TOC,
ion-exchange process and filtration

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 Dr. P. Suresh Kumar

Construction industry

Essential component in almost every step

Major role in the hydration of cement, strength, durability and curing of concrete

Quality should be similar to that of potable water

Free from impurities

(suspended solids, dissolved salts, sewage, oils & organic matter)

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 Dr. P. Suresh Kumar

High purity water quality:

Soft water

Distilled water

Deionised water

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Numerical Problems

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 Dr. P. Suresh Kumar

Q. Calculate the temporary and permanent hardness of a sample of water

containing the following impurities: Mg(HCO3)2 : 146 mg/L; Ca(HCO3)2 : 81 mg/L;
CaSO4 : 68 mg/L; MgCl2 : 50 mg/L; CaCl2 : 75 mg/L.

Solution:

Convert all of them in terms of CaCO3 eq (molar wt 100)

Temporary hardness due to Mg(HCO3)2 and Ca(HCO3)2 [molar weight of Mg(HCO3)2
and Ca(HCO3)2 are 146 and 162 respectively]
Temporary hardness = 146*100/146 + 81*100/162 = 100 + 50 = 150mg/L = 150 ppm

Permanent hardness due to CaSO4 , MgCl2 and CaCl2 [molar wt 136, 95 and 111
respectively]
Hence permanent hardness = (68*100/136) +(50*100/95) + (75*100/111)
= 50+52.63 +67.56 = 170.19 mg/L = 170.19 ppm

Total hardness = 150 + 170.19 = 320.19 ppm

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 Dr. P. Suresh Kumar

Q. 1.0 g of CaCO3 was dissolved in dil HCl and diluted to 1000 mL. 20 mL of
this solution required 23.0 mL of EDTA solution for titration. 40 mL of a hard
water sample required 18 mL of EDTA solution for titration. 40 mL of same
hardwater on boiling, filtering etc required 12 mL of EDTA solution. Calculate
different kinds of hardness.

Solution:

1000 mL std hard water = 1.0 g CaCO3 = 1000 mg CaCO3

1 mL std hard water = 1 mg CaCO3 eq
23.0 mL EDTA = 20 mL std hardwater
1 mL EDTA = 20/23.0 mg of CaCO3 eq
40 mL sample water = 18 mL EDTA = 18* 20/23.0 mg CaCO3
1 L sample water = 18 * 20/23.0 * 1000/40 = 391.3 mg CaCO3 = 391.3 ppm (total
hardness)
40 ml boiled water = 12 mL EDTA = 12*20/23 mg CaCO3 eq
For 1 L boiled water = 12*20/23 * 1000/40 = 260.86 ppm (permanent hardness)
temporary hardness = 391.3 – 260.86 = 130.44 ppm
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 Dr. P. Suresh Kumar

Q. Calculate hardness of a water sample whose 100 ml required 20 ml EDTA. 20

ml of CaCl2
solution whose strength is equivalent to 1.05 g of CaCO3 per liter required 30 ml
EDTA.

Solution:

1 L std hard water = 1.05 g CaCO3 eq/L

1 mL std water = 1.05 mg CaCO3 eq

20 mL std water = 30 ml EDTA
1 mL EDTA = 20/30*1.05 mg CaCO3 eq

100 mL sample water = 20 mL EDTA = 20*20/30 * 1.05 CaCO3 eq = 14 mg CaCO3 eq

1 L sample water = 14*10 mg = 140 ppm

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 Dr. P. Suresh Kumar

Q. 250 mL of water is boiled for half an hour and filtered. The filtrate is made
up to 250 mL. with distilled water. 50 mL of this water required 4 ml of 0.02 M
EDTA solution with an NH4OH-NH4Cl buffer and EBT indicator. Calculate
permanent hardness of the sample.

Solution:

Vsample * Ssample = VEDTA * SEDTA

Ssample = VEDTA * SEDTA /Vsample = 4*0.02/50 = 1.6x10-3 M

= 1.6x10-3 * 100 g/L = 160 mg/L = 160 ppm

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 Dr. P. Suresh Kumar

Q. 0.01 g of CaCO3 dissolved in water to which HCl was added required 22

mL of EDTA. 100 mL of hard water required 26 ml of EDTA. 100 mL of the
same sample of water after boiling and filtering required 18 mL of EDTA. Find
out the carbonate and non-carbonate hardness of water.

Solution:

22 mL EDTA = 0.01 g CaCO3 eq = 10 mg

1 mL EDTA = 10/22 mg CaCO3 eq
100 mL hard water = 26 mL EDTA
1 L hard water = 10*26 mL EDTA = 10*26*10/22 mg CaCO3 eq
= 118.18 mg CaCO3 eq = 118.18 ppm (total hardness)
100 ml boiled water = 18 mL EDTA
1 L boiled water = 10*18*10/22 mg CaCO3 eq = 81.8 ppm (permanent hardness)
Non carbonate hardness = Permanent hardness = 81.8 ppm
Carbonate hardness = Temporary Hardness = 118.18-81.8 = 36.38 ppm

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 Dr. P. Suresh Kumar

Q. If 20 mL of hard water sample consumes 35 mL of 0.01 M EDTA, find the

hardness of water Sample.

Solution:

Vsample * Ssample = VEDTA * SEDTA

Ssample = 35*0.01/20 = 0.0175

Weight in sample = 0.0175*100 g/L

= 1.75 g/L = 1750 mg/L = 1750 ppm

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Q. The hardness of 1,00,000 liters of a sample of water was completely removed

by passing it
through a zeolite softner. The softner then required 400 litres of NaCl solution
containing 100 g/L of NaCl for regeneration. Calculate the hardness of the
water.

Solution:

1 L NaCl = 100 g
400 L NaCl = 400*100 = 40,000 g

CaZ+2NaCl →CaCl2 +Na2 Z

100 parts of CaCO3 = 2*58.5 parts of NaCl
50 parts of CaCO3 = 58.5 parts of NaCl
CaCO3 eq of 40,000 g NaCl = 40,000x50/58.5 g = 34,188 g
1 L of hardwater => 34,188/1,00,000 g CaCO3
= 0.3419 g = 341.9 mg CaCO3 = 341.9 ppm
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 Dr. P. Suresh Kumar

Q. A completely exhausted zeolite softner requires 120 litres of NaCl soln having
100 g/L of NaCl. How many litres of water having a hardness of 500 ppm can be
softened by the zeolite?

Solution:

1 L NaCl = 100 g
120 L NaCl = 120*100 g = 12,000 g
50 parts of CaCO3 = 58.5 parts of NaCl

CaCO3 eq of 12,000 g NaCl = 12,000*50/58.5 = 10,256.41 g = 1,02,56,410 mg CaCO3

hardness of water = 500 ppm
No. of liters of sample that can softened = 10256410/500 = 20512.8 L

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 Dr. P. Suresh Kumar

Q. A zeolite softner is 80 % exhausted when 5,000 L of hardwater was passed

through it. The
softner required 20 L of NaCl solution of strength 150 g/L of solution.
Calculate the hardness of water sample.

Solution:
1 L NaCl = 150 g
20 L NaCl = 20*150 = 3000 g
CaZ+2NaCl →CaCl2 +Na2 Z
100 parts of CaCO3 = 2*58.5 parts of NaCl

50 parts of CaCO3 = 58.5 parts of NaCl

CaCO3 eq of 3000 g NaCl = 3000x50/58.5 g = 2564.1 g

1 L of hardwater => 2564.1/5,000 g CaCO3 = 0.5128 g = 512.8 mg CaCO3

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 Dr. P. Suresh Kumar

Q. A completely exhausted zeolite softener requires 25 L of NaCl solution

having 100 g/L of NaCl. How many litres of water having hardness of 250 ppm
can be softened by the zeolite?

Solution:
1 L NaCl = 100 g
25 L NaCl = 25*100 g = 2500 g
50 parts of CaCO3 = 58.5 parts of NaCl

CaCO3 eq of 2500 g NaCl = 2500*50/58.5 = 2,136.752 g = 2136752 mg CaCO3

Hardness of water = 250 ppm
No. of liters of sample that can softened = 2136752/250 = 8547 L

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Q. Ten thousand liters of hard water was made soft with zeolite. The
exhausted zeolite required a total amount of 8 liters of NaCl solution
containing 150 g/L for regeneration. Calculate the hardness of water.

Solution:
1 L NaCl = 150 g
8 L NaCl = 8*150 g = 1200 g
50 parts of CaCO3 = 58.5 parts of NaCl

CaCO3 eq of 1200 g NaCl = 1200*50/58.5 = 1025.641 g = 10,25,641 mg CaCO3

Per liter of sample = 1025641/10,000 = 102.56 mg
Hardness of the water = 102.56 ppm

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 Dr. P. Suresh Kumar

Q. An exhausted zeolite softer was regenerated by passing 250 liters of NaCl

solution having a strength of 120 g/L. If the hardness of the sample water is 400
ppm, calculate the total volume of the hardwater that has been softened in the
zeolite softer.

Solution:
1 L of NaCl = 120 g
250 L of NaCl = 250*120 g
50 parts of CaCO3 = 58.5 parts of NaCl

CaCO3 eq of 250*120 g of NaCl = 250*120*50/58.5 g = 25641.026 g = 25641026 mg

Hardness of the water = 400 ppm
Number of liters of water purified = 25641026/400 = 64102.56 L

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