POST GRADUATE PROGRAM

Design of experiment and analytical techniques

Critic on:- cationization of cotton with ovalbumin to
improve Dyeing of modified cotton with cochineal
natural dye

Worku Tegegene
First Year MSc. in Textile Chemistry

Submitted to: Ass. Professor. Million A.

February ,2021.
 1. Introduction

fiber–dye bonding
Cochineal natural dye
Ovalbumin :-egg white, extracted from a scale insect,
Cationization red dye

carminic acid ,
anthraquinone,
plain weave cotton fabric Ovalbumin

Citric acid and DMDHEU:-

cross linkers

Carminic acid powder

iron(II) sulfate,
Potassium alum
ovalbumin and cross-linker concentrations and for
the dyeing temperature ,

Kinetic and equilibrium data

thermodynamic parameters of dyeing.

Fastness
2.Selection of response variables/levels
The factors /variables with their levels are

Ovalbumin concentration (g /L) 50 150

Dyeing temperature (C) 55 85

DMDHEU concentration (g/ L) 30 90

 In choosing the responses, only the amount of dye

adsorbed are considered.
 Con…
but there are different responses regarding to the
treated fabric by different cross linking agents like color
strength &tensile strength

In my opinion it is also better to use more factors or

variables in order to get the optimal response values like
PH and time by keeping constant LR
 3. Choice of experimental design
 In this journal , statistical experimental design was
adopted using complete factorial design

A statistical experimental design was adopted using 23

complete factorial design because it is the most efficient,
simple to study of the effects of two or more factors

So ,For 3 factors it is better to use factorial designs

because all possible combinations of the levels of the
factors are investigated as a result I appreciate the
authors by using full factorial design
4. Model significance and model adequacy,
fit statistics, regression analysis
In Estimating factor effects, A – ovalbumin concentration
B – DMDHEU concentration
C - temperature
AB –interaction
AC- interaction
BC- interaction
ABC- interaction

The effect estimates are:

A = 11.87 ,B = 3.02 , C= -3.47, AB=0.82,AC=0.42 , BC=-0.37
ABC=- 0.52
 CON…
The regression model
q = 9.93905 + 0.118669A + 0.050382B – 0.115754C

Degrees of
Freedom
Source Sum of squares Mean square F-value P-value

Model 324.04 3 108.01 219.12 <0.0001

A - Ovalbumin concentration 281.65 1 281.65 571.36 <0.0001

B - DMDHEU concentration 18.28 1 18.28 37.08 0.0009

C - Temperature 24.12 1 24.12 48.93 0.0004

Curvature 0.0518 1 0.0518 0.1051 0.7568

Lack of fit 2.55 4 0.6379 3.14 0.2558

Pure error 0.4061 2 0.2031 – –

Total 327.05 10 – – –
 CON…
From the regression model ,the interaction effects
AB,AC, BC , ABC and error are not mentioned but the
general form of regression model should include all the
factors and errors unless if it is insignificant

The F-test for the “model” source is testing the

significance of the overall model; that is, is either A, B,
C,AB,AC,BC or ABC of these effects is important.

F value is a value on the F distribution that can be used

to determine whether the test is statistically significant.
So it is statistically significant based on the model
 5. Statistical analysis

P-values lower than 0.05 indicate that the model and

the terms are statistically significant.

The values of the terms A, B, C showed that P-value

<0.05, indicating that these terms produce significant
effects in the model

however the author didn’t explain the interaction

effects with its statistical significance like AB,AC,BC,ABC
and also he didn’t explain the relation b/n factors and
responses
 CON…
Model equation R2 adjusted R2
predicted
q =9.93905 + 0.118669A + 0.050382B – 0.115754C 0.9864 0.9660
 CON…
To understand the interaction of the components
and estimate the efficiency of cationized cotton dyeing
parameters over independent variables, three
dimensional (3D) response surface curves were plotted
The increased concentration of ovalbumin in the
solution is related to the higher protein content on the
fabric surface. more amine groups onto the cotton fiber
surface dye adsorption sites.

High dyeing temperatures promotes the weakening

of the attractive forces, there is a reduction in the
affinity of the dye , dyeing process is exothermic
 CON…
The direct influence of the concentration of the
DMDHEU cross-linker on the padding solution in the
increase of the dye adsorption N-methylol groups which
during the cross-linking bind with both the cellulose and
ovalbumin

However in order to show the model adequacy, actual

Vs predicted graph should be plotted but In this journal
it is not mentioned
 6. Re-design
The factors /variables with their levels are
Ovalbumin concentration (g /L) 50 150

Dyeing temperature (C) 55 85

DMDHEU concentration (g/ L) 30 90
Dyeing time (min) 50 60

PH 3 5

LR keep constant @ 1:50

 CON…
The responses that has to be redesigned are

The amount of dye adsorbed (mg/g)

The colour strength( K/S)

The tensile strength (N/tex)

A statistical experimental design was adopted

using 25complete factorial design