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Test Method To Check The

Concentration of Caustic &


Silica in Peroxide Bleach Bath

Introduction
1.
2.
3.
4.
5.
6.

Hydrogen Peroxide is most widely used Bleaching


Agent for more than 85% of Textile Substrate.
Process involves the the treatment of material with a
solution of H2O2 in alkaline media.
The active bleaching agent is HO2The colored substances in the material are oxidized.
It produces a stable white color, and bleached
fabrics are highly hydrophillic.
It produces Non Toxic reaction products.

What is Cross
Checking ?
It is process in which we examine the concentration of
caustic and silica in peroxide bleach bath at regular
intervals of time so as to make the the process more
efficient and decrease the degradation of material under
treatment.

Why It is Required ?
H2O2 H+ + HO2The above reaction is activated in alkaline media and is
reversible. Alkali shifts the reaction to right hand by absorbing
the proton.
H+ + HO2- HO2- + H2O (in presence of OH- )
An increase in amount of alkali will increase the rate of
formation of HO2- , thereby leading to degradation of material &
a decrease will result in decreased bleaching efficiency.
The pH range preferred is 10.4 to 10.8 , because
1. It is Safe &
2. Rate of formation of HO2- is equal to rate of its consumption
for bleaching.

Effect of pH on Decomposition of H2O2


pH

% decomposition of H2O2

10.4

11.1

13.5

11.8

19.0

12.2

25.0

12.6

59.2

Why Silica for stabilization?


The HO2- is very unstable & it can be stabilized by inserting a cation
with high charge density like Mg , but it suffers a problem of
precipitation in strongly alkaline media. Therefore silica is used which
makes six-chain structure for stabilization.

Note: Silica also


controls the
decomposition of
H2 O 2

Test Method 1
Principle : Silica reacts with Sodium Fluoride in
the presence of water to form caustic soda as
under:
SiO2+ 6NaF + 2 H2O Na2SiF6+ 4NaOH

Reagents Required
H2SO4: 0.1 N Standardized with NaOH
Sodium Fluoride
Methyl Red
Methylene Blue

Indicator to be Used
0.1 gm of Methylene Blue is dissolved in 100
ml of Distilled Water.
0.2 gm of Methylene Red is dissolved in 100
ml of Ethyl Alcohol.
The above two solutions are mixed and this
solution is used as Indicator.
The end point is shown by change in color
from Green Purple

Procedure
Take 10 ml of the peroxide solution in 250 ml flask.

Add 100 ml distilled water

Add five drops of Indicator & titrate with N/5 Sulphuric Acid Solution

Let the reading be A

Add 0.1 gm of Sodium Fluoride

Shake for 1 Minute

Titrate again

Let reading be B

Continued.

Also find the volume of N/5 Sulphuric Acid required to neutralised 1 gm of Sodium
Fluoride.

Let this reading be C

Calculations
(A-X) x N x 0.040 x100
10
Percent Silica: {B-(A+C)} x N x 0.060 x 100
4 x 10
X : {B-(A+C)} x 60 x D
4 x 31
Where , N = Normality of acid
D = Ratio of Na2O:SiO2 of the sodium silicate
used in the bath.
This test method is very accurate in estimating the alkali in peroxide bath
except the case that Phosphates & Borates are present which affect the test
accuracy.

Percent NaOH :

Test Method 2 : AATCC 98-2002


This test method determines the total alkali content of
bleach bath containing Hydrogen Peroxide.
Principle: A weighed specimen of the bleach bath is
titrated with a standardized solution of Sulphuric Acid
to a Phenol Red end-point . The total alkali content is
expressed as %NaOH.

Reagents Required
Phenol Red i.e. , Phenol- Sulphonphthalein.
H2SO4 (0.1 N)

Caution : Water should not be added to acid.


Acid should be added to water for
dilution.

Procedure
Weigh 10gm of specimen from bleach bath & add 20 ml of water to
it.

Add 2-3 drops of Phenol Red solution.

Titrate against 0.1N H2SO4 to a Greenish Yellow end-point.

Let this reading be Y

Repeat the experiment to get three concordant readings.

Calculations
% Total Alkali, as NaOH: Y x N x 0.040 x 100
W
Where, N = normality of H2SO4,
0.040 = milliequivalent weight of NaOH ,
W = mass of specimen

New Developments in
Determination Caustic & Silica
Numerous attempts have been made to replace the manual
titration by an automatic titration where end point was not
determined by visual color change but via a potential change at
redoxelectrodes.
Such systems were based on :
Calorimetric
Potentiometric
Conductometric methods of determination.
The main drawbacks in these systems were:
High Investment Cost
Long Response Time( of order of minutes)

FIA System
The Flow Injection Analysis(FIA) was developed which
have a short response time (In seconds). This system is
based on spectrophotometric detection.
A constant flow of the bleaching solution(Flow) is mixed
with a constant flow of solution of known Concentration
of Caustic(Injection). This solution is detected and a
correct pH is adusted and liquor is fed to machine. The
process is continuous and adjust the pH after regular
intervals of time.

Sensors

Conclusion
Therefore, We can say that the pH control is the most
important parameter in Peroxide Bleaching. We have to
control this parameter by checking the amount of alkali
present in bath at regular intervals. This can be done either
by titration method or by Automatic Sensing Instruments.
With FIA system , the concentration of Hydrogen Peroxide as
well as pH can be determined over complete pH area ,
although the setup cost is very high.

References
Process & Quality by ATIRA
AATCC Testing Manual
Analytical Electrochemistry in Textiles by P. Westbroek

Thank You