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CY8292 –CHEMISTRY FOR TECHNOLOGISTS

UNIT – 4 CHEMICALS AND AUXILIARIES

LECTURE PLAN

4.1) Introduction to auxiliaries

4.2) Preparation, properties, uses of Bleaching powder

4.3) Preparation, properties, uses of sodium hypochlorite

4.4) Preparation, properties, uses of Hydrogen peroxide

4.5) Preparation, properties, uses of chlorine dioxide

4.6) Estimation of available chlorine in hypochlorite bleach liquor

4.7) Determination of strength of hydrogen peroxide

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 CY8292 –CHEMISTRY FOR TECHNOLOGISTS

UNIT – 4 CHEMICALS AND AUXILIARIES

4.1) INTRODUCTION TO AUXILIARIES

An auxiliary is defined as a chemical product which enables a processing operation to be

carried out more effectively. In textile industry, the operation may be preparation, dyeing,
printing or finishing. (e.g) Bleaching agents, wetting agents

Functions of auxiliaries:

(a) To prepare the substrate for coloration (e.g) bleaching agents, wetting agents
(b) To protect the substrate from the effects of temperature, operating conditions
(c) To modify the sorption characteristics of colorants (eg) accelerators, retarders
(d) To stabilise the medium by improving dye solubility
(e) To improve the fastness of dyeing
classification of auxiliaries:

(i) Non surfactants (eg) electrolytes, acids and bases

(ii) Surfactants (eg) cationic, anionic, non-ionic surfactants
Applications of auxiliaries and surfactants :

In consumer goods In industries

Shampoos Heavy oil recovery

Dish detergents Ore flotation

Laundry detergents Dry cleaning

Fabric softeners Water repellency

Conditioners Pesticide and herbicide applications

Diapers Emulsification process

Contact lens cleaners Solubilisers

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4.2) PREPARATION, PROPERTIES & USES OF BLEACHING POWDER:

Bleaching powder is represented by the formula CaOCl2. Bleaching powder is also known
as Chloride of lime, calcium oxy chloride, Calcium hypochlorite.
When slaked lime Ca(OH)2 reacts with chlorine, it forms bleaching powder.
Ca(OH)2 + Cl2  CaOCl2 + H2O

Synthesis of bleaching powder

BACHMANN’S PROCESS (Modern method)

1. The chlorinating tower is made up of cast iron.

2. It has two inlet pipes at bottom to send chlorine gas and hot air.
3. One outlet pipe is provided at the top to expel waste and unreacted chlorine gas.
4. The tower contains number of trays with rotating rakes.
5. Through the top side hopper, slaked lime is added slowly and moved down by rotating
rakes.
6. This lime meets up the upcoming chlorine gas to form CaOCl2. This is known as
“Principle of counter currents”.
7. It is collected at the barrel kept at the bottom.
8. Hot air is used to drive away unreacted chlorine gas.
9. Reaction: Ca(OH)2 + Cl2  CaOCl2 + H2O

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HASENCLEVER METHOD (Old process):

Hasenclever plant contains a number of horizontal cylinders with rotating shafts and
blades. From the top hopper, slaked lime is added. The lime is moved down slowly by the
blades. Simultaneously chlorine gas is passed up in opposite direction. This is known as
“Principle of counter currents”. The downward lime and up going chlorine are reacting
completely and the product is produced. The product bleaching powder is collected in the
receiver kept at the bottom.
Reaction: Ca(OH)2 + Cl2  CaOCl2 + H2O

PHYSICAL PROPERTIES OF BLEACHING POWDER:

1. Bleaching powder is yellowish white powder with strong smell of chlorine.

2. It is soluble in cold water.

CHEMICAL PROPERTIES OF BLEACHING POWDER:

1. Decomposition
2. Reaction with excess quantity of acids
3. Reaction with minimum quantity of acids
4. Oxidising nature
5. Bleaching property

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1. Decomposition:

The bleaching powder on exposure to atmosphere, it reacts with the atmospheric CO2 and
liberates Chlorine gas.
CaOCl2 + CO2  CaCO3 + Cl2

2. Reaction with excess quantity of acids:

With excess quantity of acids, bleaching powder liberates the whole of chlorine present in it.
The amount of chlorine set free here is called available chlorine. Bleaching powder is priced
according to the amount of available chlorine. Normally it ranges from 35 – 38%.
CaOCl2 + H2SO4  CaSO4 + H2O + Cl2

3. Reaction with minimum quantity of acids:

Bleaching powder liberates nascent oxygen in presence of small amount of dilute acids.
This is the reason for its oxidizing and bleaching property.
2 CaOCl2 + H2SO4  CaCl2 + CaSO4 + 2 HCl + 2 [ O ]

4. Oxidising properties:

a) It oxidizes potassium iodide into iodine in presence of hydrochloric acid.

CaOCl2 + 2 KI + 2 HCl  2 KCl + I2 + H2O + CaCl2
b) It oxidizes sodium arsenite into sodium arsenate.
CaOCl2 + Na3AsO3  CaCl2 + Na3AsO4
c) It oxidizes lead oxide to lead di oxide, manganese oxide to manganese di oxide.
CaOCl2 + PbO  CaCl2 + PbO2
CaOCl2 + MnO  CaCl2 + MnO2

5. Bleaching properties:

The bleaching property of bleaching powder is more effective in acidic medium. The nascent
oxygen [O] liberated from the bleaching powder converts coloured fabric into colourless
fabric.
2 CaOCl2 + H2SO4  CaCl2 + CaSO4 + 2 HCl + 2 [ O ]
Coloured Fabrics + [ O ]  Colourless fabrics
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Mechanism of bleaching action:

The bleaching agents are used to remove stains in clothing. The stain colours are due to the
presence of multiple bonds in organic molecules. These bonds absorb and emit visible
electro- magnetic radiation. When bleaching agents come in contact with these organic
molecules, they oxidize them forming new products. These new products no longer have
multiple bonds , hence it looks white or completely vanishes.

APPLICATIONS OF BLEACHING POWDER:

1. Bleaching powder is used in paper industry to bleach wood pulp.

2. Bleaching powder is used in sugar industry to bleach sugar cane juice.
3. It is available in the trade name of “Perchloron”.
4. It is used in textile industry to bleach Linen and cotton materials.
5. It is used as disinfectant and germicide in swimming pools.
6. It is used in preparation of chloroform.
7. It is used to prevent excessive shrinkage of wool during processing.

Disadvantages of bleaching powder:

1. It affects delicate fabrics like wool, silk and hair.

2. On long standing, its available chlorine decreases due to decomposition. This affects
bleaching powder quality.

Differences between Bleaching powder and Sodium hypochlorite

S.No Bleaching powder (CaOCl2) Sodium hypochlorite (NaOCl)

1 It is prepared by Bachmann’s method. It is prepared by Electrolysis of NaCl.

2 It is effective in acidic medium. It is effective alkaline medium.
3 Compared to NaOCl, less corrosive and In solution, it is corrosive. At higher
user friendly. concentration, its splashes can cause skin
burns.
4 Shelf life is comparatively moderate. Shell life is poor.
5 Its deterioration is slow. It undergoes rapid deterioration.
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4.3) PREPARATION, PROPERTIES & USES OF SODIUM HYPOCHLORITE:

Preparation by NaCl electrolysis:

1. NaOCl is prepared by the electrolysis of NaCl solution at 24 oC.
2. This electrolysis of NaCl solution liberates NaOH at cathode and Cl2 at anode.
3. These NaOH and Cl2 react together to form sodium hypochlorite.
Reaction: 2 NaOH + Cl2  NaCl + NaOCl + H2O
Construction of electrolytic bath:
1. The setup contains two rectangular vessels A and B, made up of semi-porcelain material.
2. The vessel A contains 25 – 30 graphite electrodes joined in series.
3. The end electrodes are connected with the positive and negative terminals of a power
supply.
4. This vessel A is placed in the outer vessel B, containing pure NaCl solution.
5. Now, the Brine (NaCl) solution is filled in both A and B vessels.
6. To maintain the temperature below 24oC, cold water is circulated through a cooling coil
immersed in vessel B.
7. On passing current, NaOH and H2 are formed on the cathodes.
8. Cl2 is liberated at anode.
9. This NaOH and Cl2 are reacting together to form a mixture of NaOCl and NaCl.
10. This mixture is known as bleaching mixture, from which NaOCl can be separated out.

PHYSICAL PROPERTIES OF SODIUM HYPOCHLORITE:

1. Sodium hypochlorite is pale greenish liquid.
2. It is also known as soda bleach or liquid bleach.
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CHEMICAL PROPERTIES OF SODIUM HYPOCHLORITE:
1. Auto oxidation & oxidation
2. Decomposition
3. Reaction with excess quantity of acids
4. Reaction with minimum quantity of acids
5. bleaching property

1. Auto oxidation & oxidation

It undergoes auto oxidation at high temperature to form sodium chlorate.
3NaOCl  NaClO3 + 2 NaCl
It oxidizes sodium arsenite into sodium arsenate.
NaOCl + Na3AsO3  NaCl + Na3AsO4

2. Decomposition
It undergoes decomposition. The decomposition is slowed down by the presence of sodium
hydroxide.
2 NaOCl  2 NaCl + O2

3. Reaction with excess quantity of acids

With excess quantity of acids, sodium hypochlorite liberates the whole of chlorine present
in it. The amount of chlorine set free here is called available chlorine. Bleaching powder is
priced according to the amount of available chlorine. Normally it ranges from
35 – 38%.
NaOCl + 2HCl  NaCl + H2O + Cl2

4. Reaction with minimum quantity of acids

Soidum hypochlorite liberates hypochlorous acid (HOCl) in presence of small amount of
dilute acids.
2 NaOCl + H2SO4  Na2SO4 + 2 HOCl

5. Bleaching property
Soidum hypochlorite liberates hypochlorous acid (HOCl) in presence of small amount of
dilute acids. HOCl is thermodynamically unstable and undergoes decomposition on fabric
to form hydrogen chloride and nascent oxygen. This nascent oxygen is causing bleaching
action.
2 NaOCl + H2SO4  Na2SO4 + 2 HOCl
HOCl  HCl + [O]
Coloured Fabrics + [ O ]  Colourless fabrics
USES OF SODIUM HYPOCHLORITE:
1. It is used as a disinfectant, because of its ability to oxidize the cell membranes of bacteria.
2. It is used as deodourant in dairies.
3. It is used in sewage disposal and water supplies.
4. It is used as a bleaching agent in textile industries. 8
4.4) PREPARATION, PROPERTIES & USES OF HYDROGEN PEROXIDE
Hydrogen peroxide is represented as H2O2.
Industrial synthesis of H2O2 by Electrolysis of sulphuric acid

Setup:
1) 60% H2SO4 solution is taken in a large test tube.
2) The test tube is kept inside an ice cooled beaker.
3) An electrolytic cell is constructed inside the test tube.
4) In electrolytic cell, a platinum wire sealed in a glass tube is taken as anode.
5) A copper wire, coiled around the glass tube is taken as cathode.
6) The anode and cathode are electrically connected and 2 amp current is passed.
Reactions:
7) This current causes electrolysis of H2SO4. It splits into H+ cation and bisulphate anion.
-
H2SO4  H+ + HSO4
8) At cathode, H+ ion is getting reduced and liberated as hydrogen gas.
-
2H+ + 2 e  H2↑
9) At anode, bisulphate ions combine together to form persulphuric acid (Marshall’s acid).
- - -
HSO4 + HSO4  H2 S2 O8 + 2 e
10) The persulphuric acid is further hydrolysed to produce H 2O2.
H+
H 2 S2 O 8 + 2 H 2 O  mixture of (H2O2 + 2 H2SO4)
From this mixture, H2O2 is separated by distillation. Concentration of H2O2 should be done
with utmost care as the impurities present in the solution may catalyse the explosive
decomposition of peroxide.30% H2O2 can be achieved with simple evaporation technique.
Upto 90% H2O2 is obtained by low pressure distillation. The 90% H 2O2 when subjected to
continuous crystallization yields 95 – 98% H2O2.
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Laboratory preparation:
1. From peroxides:
When sodium peroxide or barium peroxide is treated with ice cold 20% sulphuric acid
solution, it results in the formation of hydrogen peroxide.
Na2O2 + H2SO4  Na2SO4 + H2O2
BaO2 + H2SO4  BaSO4 + H2O2
2. From antrhaquinol:
When 2-alkyl anthraquinol is oxidized, it forms alkyl anthraquinone and hydrogen peroxide.

3. From Propanol:
When propanaol is oxidized, it forms acetone and hydrogen peroxide.
(CH3)2 – CH – OH + O = O  CH3 – CO – CH3 + H2O2
CHEMICAL PROPERTIES OF H2O2:
It is a colourless, odourless, syrupy liquid.
1. Decomposition
2. Reducing properties
3. Oxidising properties
4. Bleaching properties

1. Decomposition:

Pure H2O2 is unstable and decomposes on standing or on heating.

2H2O2  2H2O + O2
This decomposition is accelerated by positive catalyst like MnO 2.This decomposition can be
delayed by using a negative catalyst like dilute H2SO4.

2. Reducing properties:

It reduces silver oxide into silver.

H2O2 + Ag2O  2 Ag + H2O + O2

3. Oxidising properties:

In presence of minimum quantity of acids, it produces nascent oxygen. This shows it has
oxidation and bleaching properties.
H+
H2 O2  H2 O + [ O ]

a) It oxidizes potassium iodide into iodine in presence of hydrochloric acid.

H2O2 + 2 KI + 2 HCl  2 KCl + I2 + 2H2O
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b) It oxidizes sodium arsenite into sodium arsenate.
H2O2 + Na3AsO3  H2O + Na3AsO4

c) It oxidizes black coloured lead sulphide into white colour lead sulphate.
4 H2O2 + PbS (black)  PbSO4 (white) + 4 H2O

4. Bleaching properties:

In presence of minimum quantity of acids, it produces nascent oxygen. This shows it has
oxidation and bleaching properties.
H+
H2 O2  H2 O + [ O ]

Coloured Fabrics + [ O ]  Colourless fabrics

H2O2 is used to bleach straw, glue, textiles. Fats and oils, silk, wool, hair, leather etc.,

Mechanism of bleaching action:

The bleaching agents are used to remove stains in clothing. The stain colours are due to the
presence of multiple bonds in organic molecules. These bonds absorb and emit visible
electro- magnetic radiation. When bleaching agents come in contact with these organic
molecules, they oxidize them forming new products. These new products no longer have
multiple bonds , hence it looks white or completely vanishes.

USES OF HYDROGEN PEROXIDE

1. It is used as bleaching agent for delicate materials like wool, silk, hair and leather.
2. It has good oxidation and power generation capacity.
3. It is used as antiseptic for washing wounds.
4. It is used as rocket propellant.
5. It is used to restore the faded colours of black lead paints into its original black colour.
6. It is commercially available in the trade name of “Perhydrol” which effectively works in
alkaline medium.

ADVANTAGES OF HYDROGEN PEROXIDE OVER OTHER CHLORIDE

BLEACHING AGENTS:

1. It is universal bleaching agent for almost all type of fabrics.

2. Its loss in weight during bleaching process is minimum.
3. It is easily absorbed by fabric.
4. The extent of fabric degradation by this bleach is low.
5. Yellowing tendency after the process is minimum when compared to hypochlorites. 11
4.5) PREPARATION, PROPERTIES & USES OF CHLORINE DIOXIDE (ClO2)
(Note - ClO- is Hypochlorite. ClO2- is Chlorite. ClO3- is Chlorate. ClO4- is Perchlorate)

Laboratory preparation:
1. From Sodium chlorite:
When sodium chlorite and chlorine gas are reacting with each other, it results in
chlorine dioxide.
2 NaClO2 + Cl2  2 ClO2 + 2 NaCl
This reaction is favoured by two conditions:
i) Presence of strong acid (eg) H2SO4 ii) Presence of a reducing agent (eg) Methanol

2. From Potassium chlroate:

When potassium chlorate is heated with conc. Sulphuric acid, it forms chlorine di oxide
(ClO2), potassium bisulphate (KHSO4) and perchloric acid (HClO4).
3 KClO3 + 3 H2SO4  3KHSO4 + HClO4 + H2 O + 2 ClO2

3. From Silver chlorate:

When dry chlorine is passed over silver chlorate (AgClO 3) at 90oC, it forms chlorine
90oC
dioxide.
2 AgClO3 + Cl2  2ClO2 + 2 AgCl + O2

PHYSICAL PROPERTIES OF CHLORINE DIOXIDE:

1. It is dark yellow pungent smell gas.
2. On condensation it forms dark red liquid.
3. The liquid on crystallization , it forms orange red crystals.
4. It is stable in dark, but decomposes in light.
5. On heating it explodes violently.
CHEMICAL PROPERTIES OF CHLORINE DIOXIDE:
1. Decomposition
2. Explosion
3. Action with water
4. Oxidising properties
5. Bleaching properties
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1) Decomposition
Both solid and liquid ClO2 are slowly decomposed in dark, but on exposure to light, they
decompose rapidly to produce nascent oxygen.
ClO2  ClO + [ O ]
2) Explosion:
a) ClO2 liquid explodes above 40oC.
b) The gas explodes by an electric spark and gives chlorine and oxygen.
2ClO2  Cl2 + 2 O2
c) Sulphur, phosphorus compounds spontaneously catch fire in gaseous ClO 2.
3)Action with water:
ClO2 dissolves in water and gives a mixture of chlorus acid (HClO 2) and chloric acid.
(HClO3)
2 ClO2 + H2O  HClO2 + HClO3
4) Oxidising properties:
On exposure to light, ClO2 decompose rapidly to produce nascent oxygen. This shows ,
ClO2 can act as bleaching and oxidizing agent.
ClO2  ClO + [ O ]
It oxidizes phenol to quinone and maleic acid.
5) Bleaching properties:
On exposure to light, ClO2 decompose rapidly to produce nascent oxygen. This shows ,
ClO2 can act as bleaching and oxidizing agent.
ClO2  ClO + [ O ]
Coloured Fabrics + [ O ]  Colourless fabrics
USES OF CHLORINE DIOXIDE:
1. ClO2 is used in water purification.
2. ClO2 is used in mollusk control.
3. ClO2 is used for bleaching the highest grade paper pulp and textiles.
4. It is used to improve the quality of low grade fats and oils.
5. It is used to make wool unshrinkable.
6. It produces brighter, stronger fiber than chlorine bleach and thus acts as food additives.
7. It does not form environmentally harmful chlorinated byproducts like dioxins.
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4.6) ESTIMATION OF AVAILABLE CHLORINE IN HYPOCHLORITE
BLEACH LIQUOR and BLEACHING POWDER
Aim:
To determine the percentage of available chlorine present in the given sample of
hypochlorite bleach liquor / bleaching powder.
Definition:
With excess quantity of dilute acids, bleaching powder liberates the whole of chlorine
present in it. The amount of chlorine set free here is called available chlorine. Bleaching
powder is priced according to the amount of available chlorine. Normally it ranges from
35 – 38%.
CaOCl2 + H2SO4  CaSO4 + H2O + Cl2
NaOCl + 2 HCl  NaCl + H2O + Cl2

Significance of Available chlorine:

i) Bleaching powder is priced according to the amount of available chlorine.
ii) Normally it ranges from 35 – 38%.
iii) The lower value suggests the deterioration or decomposition of the samples on storage.
Principle:
The available chlorine in the sample is determined iodometrically. The sample is first
treated with excess of Potassium iodide in acidic medium. It liberates Iodine. On adding
starch, the liberated I2 forms blue colour complex.
CaOCl2 + 2 KI + 2 HCl  2 KCl + I2 + H2O + CaCl2
NaOCl + 2 KI + 2 HCl  2 KCl + I2 + H2O + NaCl
Starch indicator + liberated I2  Blue colour complex
When this is titrated against thio, Iodine is consumed and blue colour disappears.
I2 ( from blue complex) + 2 Na2S2O3  Na2S4O6 (colourless sodium dithionate) + 2 NaI
So, the end point is disappearance of blue colour.
Procedure:
For solid sample: “m” g sample is taken and dissolved, made upto 100 ml in a standard
measuring flask.
For liquid sample: The sample is transferred and made up to 100 ml in a standard
measuring flask. 14
1) 20ml of the made up solution is pipette out in a clean conical flask.
2) 10 ml of 10% KI and 10 ml of dil H2SO4 are added to the conical flask.
3) On adding starch indicator, the liberated I2 produces blue colour.
4) This solution is titrated against standard thio solution taken in the burette.
5) End point is the disappearance of blue colour.
6) The titration is repeated for concordance.
Diagram:

Calculation:
Volume of thio consumed (V1) = From titration
Normality of std. thio (N1 ) = Known value
Volume of bleach liquor (V2) = 20 ml
Availablechlorine = Volume of Thio X Normality of Thio x Equivalent weight of chlorine
Volume of bleach liquor
Equivalent weight of chlorine = 36.45
% available chlorine = Available chlorine X 100
Weight of sample

Result:
The % of available chlorine present in the given sample of hypochlorite liquor = ------%
15
4.7) DETERMINATION OF STRENGTH OF HYDROGEN PEROXIDE:

Aim:
To determine the strength of hydrogen peroxide in the given sample.

Definition:
The volume of oxygen liberated by one volume of H2O2 on heating is noted as the strength
of hydrogen peroxide.

Significance:
Higher the strength of hydrogen peroxide, more will be its bleaching action.
The strength of H2O2 can be determined by two methods:
i) Permanganometry
ii) Iodometry

i) Permanganometry:

Procedure
1. A known volume of the given H2O2 sample is titrated against standard KMnO4 solution ,
in presence of dilute H2SO4.
2. Until the presence of H2O2, it decolorizes the KMnO4.
3. At neutralization point, where all the peroxide is consumed, the KMnO 4 colour (Pink)
persists.
4. This appearance of permanent pink colour is taken as the end point.

Short procedure
Burette solution
Pipette solution
Additional solution
Indicator
End point
Equivalent weight
Std. Potassium permanganate
20 ml hydrogen peroxide
10 ml dil. Sulphuric acid
Self indicator
Appearance of pink colour
17 for hydrogen peroxide
16
Principle & Reaction:

5 H2O2 + 2 KMnO4 + 4 H2SO4  2 KHSO4 + 2 MnSO4 + 5 O2 + 8 H2O

Though H2O2 is an oxidizing agent, in presence of a stronger oxidizing agent like potassium
permanganate, it undergoes oxidation. It forms potassium bisulphate, manganous sulphate
and liberates oxygen. As KMnO4 is acting as self-indicator, this reaction does not need any
external indicator.

Diagram:

Calculation:
Volume of permanganate consumed (V1) = From titration
Normality of std. KMnO4 (N1 ) = Known value
Volume of peroxide (V2) = 20 ml
Strength of H2O2 = Vol.of KMnO4 X Normality of KMnO4 X Equivalent weight of H2O2
ml of peroxide sample taken
(Eq wt of H2O2 = 17)
% strength of H2O2 = (strength of peroxide x 100) / ml of peroxide sample taken
Result:
The strength of hydrogen peroxide % = -----
17
ii) Iodometry:
If the peroxide sample contains organic impurities, they affect the result of
permanganometry. In such cases, iodometry is preferred.

Principle:
In presence of Ammonium molybdate and acid catalyst, Hydrogen peroxide reacts with
excess KI and liberated I2.
H2O2 + 2 KI + 2 HCl  2 KCl + I2 + 2H2O
This liberated I2, on adding starch gives blue coloration.
Starch indicator + liberated I2  Blue colour complex
When this is titrated against thio, Iodine is consumed and blue colour disappears.
I2 (from blue complex) + 2 Na2S2O3  Na2S4O6 (colourless sodium dithionate) + 2 NaI
So, the end point of disappearance of blue colour.

Procedure:
1. A known volume of peroxide sample is taken in a conical flask.
2. To this, 10 ml of 10% KI and 10 ml of dilute hydrochloric acid are added.
3. After adding starch indicator, this sample is titrated against 0.1N Thio solution taken in
the burette.
4. The end point is disappearance of blue colour.
5. The experiment is repeated for concordance.

Short procedure
Burette solution
Pipette solution
Additional solution
Indicator
End point
Equivalent weight
Std. thiosulphate solution
20 ml hydrogen peroxide
10 ml dil. Hydrochloric acid + 10 ml KI solution
Starch
Disappearance of blue colour
17 for hydrogen peroxide

18
Diagram:

Calculation:
Volume of thiosulphate consumed (V1) = From titration
Normality of std. Thio (N1 ) = Known value
Volume of peroxide (V2) = 20 ml

Strength of H2O2 = volume of Thio X Normality of Thio X Equivalent weight of H2O2

ml of peroxide sample taken
(Eq wt of H2O2 = 17)

% strength of H2O2 = (strength of peroxide x 100) / ml of peroxide sample taken

Result:
The strength of hydrogen peroxide % = -----

19