BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association...

50
BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE D. R. M SCIENCE COLLEGE, DAVANGERE-577004 A REPORT ON UGC MINOR RESEARCH PROJECT XI PLAN ( MRP (S)-1322/11-12 KAKU033/UGC-SWRO ) ENTITLED “CHARACTERIZATION OF TREATED AND UNTREATED COTTON FIBRES” SUBMITTED TO UGC By SMT. M . P. RUPASHREE. M.Sc., M.Phill., Assistant Professor, PRINCIPAL INVESTIGATOR, UGC MINOR RESEARCH PROJECT DEPARTMENT OF PHYSICS D.R.M SCIENCE COLLEGE DAVANGERE-577004 Karnataka DECEMBER-2014

Transcript of BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association...

Page 1: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE

D. R. M SCIENCE COLLEGE, DAVANGERE-577004

A REPORT ON

UGC MINOR RESEARCH PROJECT XI PLAN

( MRP (S)-1322/11-12 KAKU033/UGC-SWRO )

ENTITLED

“CHARACTERIZATION OF TREATED AND

UNTREATED COTTON FIBRES”

SUBMITTED TO UGC

By

SMT. M . P. RUPASHREE. M.Sc., M.Phill.,

Assistant Professor,

PRINCIPAL INVESTIGATOR,

UGC MINOR RESEARCH PROJECT

DEPARTMENT OF PHYSICS

D.R.M SCIENCE COLLEGE

DAVANGERE-577004

Karnataka

DECEMBER-2014

Page 2: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Smt. M. P Rupashree. M.Sc.,M Phill., Department Of Physics

Assistant Professor D. R. M. science College

Davangere-577004

Affiliated to Davangere University

Karnataka,

DECLARATION

I do here by declare that the Minor Research Project Work

entitled “CHARACTERIZATION OF TREATED AND UNTREATED

COTTON FIBRES” submitted to UGC is based on the results of

Research work carried out by me. This project has not been

submitted elsewhere for any other Degree or Diploma.

Date:1-12-2014 Smt. M. P. Rupashree

Place:Davangere Principal Investigator

Page 3: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Prof. K. S. Eswarappa. M. A, D. R. M. science College , Davangere

Principal Affiliated to Davangere University

Karnataka, -577004

CERTIFICATE

This is to certify that the Minor Research Project Work entitled

“CHARACTERIZATION OF TREATED AND UNTREATED COTTON

FIBRES” taken under UGC-XI plan has been carried out

by Smt. M.P. Rupashree, Assistant Professor of Physics, in this

Institution, in collaboration with Department of Studies in

Physics, University of Mysore, Manasagangotri, Mysore &

Department of Textile Technology, Bapuji Institute of

Engineering and Technology , Davangere.

Date :1-12-2014 Prof. K. S Eswarappa

Place : Davangere Principal

Page 4: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

ACKNOWLEDGEMENT

I would like to sincerely thank various people who, during the several months in which

this endeavour lasted, provided me with useful and helpful guidance. Without their care and

consideration, this Minor Research Project entitled “Characterization of Treated and

Untreated Cotton Fibres ” would not have been materialised.

I would like to thank Major. N. Srinivasa, former principal, Prof. K.S. Eshwarappa ,

present principal of our college, who have encouraged me to take up this project and

complete it. I would like to keep on record my sense of gratitude to the UGC for providing

funds for this Project.

I would like to place on record my deep sense of gratitude to my teacher

Dr. R.Somashekar, Chairman, Department of Studies in Physics , University of Mysore,

Manasagangotri, Mysore , who encouraged me and guided me to take up this UGC funded

project and accommodated me to work in the Departmental Laboratory and to complete this

project. I am also thankful to Research Scholar Thejas Urs.G , Department of studies in

Physics, University of Mysore, for his co-operation during my work at X- Ray Diffraction

Laboratory,

I express my sincere gratitude to Prof. Y. Vrushabendrappa , Director, Bapuji Institute

of Engineering & Technology , Davangere , who gave me an opportunity to work at BIET

for this project work and Dr. K.Murugesh Babu , Chairman, Department of Textile

Technology, Bapuji Institute of Engineering & Technology , Davangere, who guided me

throughout the project by extending his collaboration to work in the Department Laboratory.

I would like to thank Prof .K.B. Ravindra BIET, Davangere, for his co-operation while

conducting experiments.

I also like to thank Dr. J. Mahadeva, Associate Professor, PES College, Mandya, who

gave me his valuable suggestions throughout this project work.

My Thanks are reserved for Prof. N. Srinivas, H.O. D. and all my colleagues of

Department of Physics and office staff of D.R.M Science College, Davangere, who were

with me in this endeavor.

I am grateful to my beloved parents, Sri. M.P. Parswanath and Smt. Jayapadma

Parswanath and my husband H.J. Poornachandra , My children, Tejas Jain, Gautam.P &

Aravind.P and my friends who have been a constant source of my inspiration.

Smt . M.P Rupashree. Principal Investigator.

Minor Research Project.

Assistant professor of Physics.

D. R. M Science College.

Davangere-577004

Page 5: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

A Report on Minor Research Project

“Characterization of Treated And Untreated Cotton Fibres”

CONTENTS Page No.

1. Introduction 1-2

2. Materials and Methods 3-7

2.1. Materials

2.2. Preparation of Sample

2.3. Pre-treatment of Cotton Fibres-. Chemical Processes

2.3.1. Desizing

2.3.2. Scouring

2.3.3. Bleaching

2.3.4. Microwave Treatment

3. X-Ray Diffraction Studies 8-19

3.1. Experimentation

3.2. Results and Discussions

3.3. Conclusions

4. Studies on Physical , Mechanical and Dyeing Properties 20-28

4.1. Structural Studies

4.2. Moisture Regain

4.3. Mechanical Properties

4.4. Dyeing Properties

4.4.1.Dyeing of Fibres

4.4.2. Dye Exhaustion Percentage Studies

4.4.3. K/ S Values

5. Conclusions 29

7. References 30

6. Photo Gallery 32-34

8. Paper Publications 36-43

Page 6: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

LIST OF PHOTOS

Sl. No. PHOTOS Page No

1 Fig.1. Chemical Structure of Cotton

1

2 Fig.2. Raw and Ginned Cotton Fibres

3

3 Fig.3. Bleached Cotton Fibre

5

4 Fig.4. Desizing

6

5 Fig.5. Hot Air Oven

6

6 Fig.6. Scouring

6

7 Fig.7. Bleaching

6

8 Fig.8. Microwave Oven

7

9 Fig.9.RinguMiniFlex II Desktop X-Ray Difractometer

17

10 Fig.10. Cotton Sample on Sample Holder of RinguMiniFlex II

Desktop X-Ray Difractometer

17

11 Fig.11. Microscope Carl ZeisAxiostar Plus

20

12 Fig.13. Longitudinal Microscopic views of cotton fibres, using

Microscope CarlZeisAxiostar Plus using100 magnification

21

13 Fig.13. Humidifier

22

14 Fig.14. Humy Tester

22

15 Fig.15. Stelometer

24

16 Fig.16. Statex Fibre fineness tester

24

17 Fig.17. Dye Bath

24

18 Fig.18. Spectro Photometer

27

19 Fig.19. Elico double beam UV-VIS

27

Page 7: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

LIST OF TABLES

LIST OF GRAPHS

Sl.No. TABLES Page No.

1 Components of Cotton Fibres 1

2 Microwave Radiation Dosage 8

3 Microstructural Parameters - Crystallite Sizes ,Lattice Strain 18

4 Moisture Regain of Raw and Bleached Cotton Fibres 23

5 Mechanical Properties:Tenacity ,% Breaking Elongation. And Finess 25

6 Dyeing Properties:Exhaustion % and Transmittance 27

7 Dyeing Properties :K/S Values 28

Sl.No. GRAPHS Page. No.

1 XRD plot for Raw Cotton Sample . 9

2 XRD plot for Bleached Cotton Sample. 10

3 XRD plot for Microwave Treated Raw-10 Cotton Sample. 11

4 XRD plot for Microwave Treated Bleached-10 Cotton Sample. 12

5 XRD plots for Raw & Raw-10 Cotton Sampleafter smoothening. 13

6 XRD plots for Bleached & Bleached-10 Cotton Samples. 14

7 XRD plots for Raw &Microwave Treated Raw Cotton Samples. 15

8 XRD plots for Microwave Treated Bleached Cotton Samples 16

Page 8: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

1. Introduction:

Cotton is cultivated in and around the southern states of India such as

Karnataka, Andhrapradesh, Maharashatra, Tamilnadu and is a major crop of several

countries. Cotton fibres belong to a family of gossypium . Cotton has been used for

more than 3000 years because of its versatility and good finished products. Cotton is

essentially pure cellulose. The Components of raw cotton are as follows.

Table.1: Components of Cotton Fibre

80-96% Cellulose

6-8% Water

0.5 - 1% Waxes and fats

0 - 1.5% Proteins

4 - 6% Hemicelluloses and pectin’s

1 - 1.8% Ash

Cellulose content of the raw cotton fibre ranges from 88 to 96 %. Cellulose is a

polymer of ß-D-glucose with a specific configuration shown in figure. The cellobiose,

repeating unit of cellulose, consist of two beta glucose molecules linked together at

the 1:4 carbon atoms. Each successive glucose unit is rotated 1800 around the

molecular axis. This gives a linear polymer chain that is almost flat therefore suitable

for fibre formation.

Figure 2 Chemical Structure of Cotton

Page 9: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

The structure- property relation of cotton is considered as an important factor in

Textile industry.

The use of radio and microwave frequency is gaining importance for industrial

applications such as Heating, drying, and other processing. The most important

advantage of using microwave is that it is non-contact or localized heating and the

heat is produced within the material. This can be much more effective than indirect

heating where the heat propagation is by heat conduction through the material. The

microwave radiation process is fast, reliable and energy saving. Microwave Radiation

of frequency 2450MHz is used in this Study.

In the present Investigation, studies were made on the influence of microwave

radiation at different time intervals on DCH-32 Cotton fibres. Studies were made on

raw and processed cotton fibres. The cotton fibres have undergone chemical

treatments such as Desizing, Scouring and Bleaching and were exposed to Microwave

radiations of frequency of 2450 MHz at different time intervals to investigate its effect

on DCH- 32 cotton fibres.

The changes in crystallite size and Lattice strain have been calculated using the

method of X-ray Diffraction (XRD). .In the present Investigation, an attempt has been

made to understand the effect of microwave radiations on Microstructural changes,

Moisture Regain and Mechanical properties such as Tenacity, Breaking Elongation,

Fineness, and dyeing behaviour of bleached DCH-32 cotton fibres.. Such property-

structural changes can be highly beneficial for the processing of Cotton fibers in fabric

industry.

Page 10: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

2. Materials and Methods

2.1. Materials:

DCH-32 cotton fibres used in this study were procured from local markets of

Davangere, Karnataka, Southern region of India. DCH-32 Cotton fibres used in this

study are Long stapled Cotton fibres of average staple length of 35mm-37mm with a

spinning count of 70’s to 80’s. These cotton fibres were developed by Agricultural

University Dharwar & are improved version of Varalakshmi Cotton Fibres. These are

also known as Davangere Cotton as they are grown in this area for a higher percentage

in Karnataka.

Chemicals used for desizing / scouring / bleaching included wetting agent,

Hydrochloric acid (0.5% concentration), Sodium Hydroxide flakes, Hydrogen

Peroxide of 100% volume 30% strength, Sodium Carbonate and Sodium Silicate and

Direct Dye.

Fig.1. Raw and Ginned Cotton Fibres

Page 11: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

2.2. Methodology:

2.3. Preparation of Sample

Raw cotton was plucked manually after ripening. This cotton was freed from

the buds & was taken for ginning. Ginning is a process where raw cotton gets

separated from seed, seed bits and other small objects. After ginning cotton was taken

for baling till it became lint. This lint raw cotton was used for this study.

2.4. Pre-treatment of cotton fibres – Chemical processes;

2.4.1.Desizing:

Desizing is the process of removing the starch present in the raw cotton fibre

which acts as a barrier for absorbing water and chemicals. The cotton fibre was

desized with 5% HCL and 3-4 drops of wetting agent using a fibre to liquor ratio of

1:40. The fibre was desized for 90 minutes at 95o C temperature. After desizing the

fibre was dried in an oven and then scoured.

Treatment of Fibres (Chemical)

Processing of Raw Cotton Fibres

Treatment of Fibres (Microwave)

Investigation of Properties of treated and untreated Cotton Fibres

Structural Studies like Crystallite Size &

Lattice Strain Using XRD

Mechanical Properties

1.Strength (Tenacity) 2 Breaking. Elongation 3.Fineness

Microstructural Studies Longitudinal View Moisture Regain

Dyeing Behaviour K/S Values Transmittance % Exhaution%

Page 12: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Calculations: Amount of H CL = Weight of fibre X ( 5% ) HCL

Amount of Liquor = Weight of fibre x 40

The weighed cotton Fibre sample was introduced into the desizing bath at room

temperature which contained 5% HCL and fibre to liquor (water) ratio of 1:40 .

Temperature of the bath was gradually increased to 95 o

c and the fibre was boiled at

this temperature for 90 minutes and then removed from the bath and dried using hot

air oven .

2.4.2. Scouring:

The process of scouring removes natural impurities such as oils, fats and

waxes, which are present in the cotton to make it absorbent towards water and dye

stuffs. The desized cotton fibre was scoured with 4% NaOH, 1% Na2CO3, and 3-4

drops of wetting agent, using fibre to liquor ratio of 1:40. The fibre was scoured for 90

minutes at 95oC temperature. After scouring the fibre was dried in an hot air oven.

The dried sample was then bleached.

2.4.3. Bleaching:

Bleaching is the process of removal of colouring matter (pigments) present in

cotton fibre and to improve the whiteness. The Scoured cotton fibre was bleached in a

bath containing 2% Na2CO3, 10ml of H2O2 (100 vol, 30%) / 1litre of water, 15g

sodium silicate / litre of water and 3-4 drops of wetting agent at 85 o

C temperature for

90 minutes. The Bleached cotton fibre was removed from bath and then dried in the

hot air oven.

Fig.2. Bleached Cotton Fibre

Page 13: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Desizing and Scouring

Fig.3. Desizing Fig.4. Hot Air Oven

Fig.5. Scouring Fig.6. Bleaching

Page 14: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

2.5. Pre-treatment of cotton fibres: Microwave treatment:

A commercially available microwave (Godrej make-20l capacity) with

frequency 2.45GHz was used in our study. This has an output power of 800watt,

which can be varied by the selection of the knob which determines the percentage of

power. The power output of the oven was set for 400watt. The Raw and bleached

cotton fibres were exposed to microwave radiations for different time intervals of

5,10,15,20 min. The dosage rate = (P x t) Gy.

Table.2. Microwave Dosage Rate

[Note: Raw-5, Bleach-5 means Raw and Bleached Cotton Fibres exposed to

Microwave Radiation for 5 min. & so on.]

Time

In minutes

Dosage Rate

In Gy

Dosage Rate

In Gy

5 5x60x400 120 KGy

10 10x60x400 240KGy

15 15x60x400 360KGy

20 20x60x400 480KGy

Desizing

Fig.7. Microwave Oven

Page 15: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

3. X-Ray Diffraction Studies

3.1. Experimental

The cotton samples of required size were taken in the sample holder of Rigaku-

miniflex II desktop X-Ray diffractometer with the settings of 30 kV and 15 mA,

scanning rate of 5o per minute, and for the range of 5

o to 40

o with step size of 0.02

o

being recorded. The integral breadth of the diffraction peaks is related to the apparent

size of the crystals and to their microstrains. If the size and strain broadening exist

simultaneously, then crystallite size and strain can be calculated by Williamson-Hall

plot (W-H plot). For relative comparison of the parameters, WH plot is a reasonably

reliable one. The W-H plot considers both limited size of the crystals and the presence

of crystallographic distortions which leads to Lorentzian intensity distributions. The

slope of the W-H plot represents the average strain in the crystal, whereas intercept

with the 𝑦-axis gives the crystallite size [12]. The Williamson-Hall relation is given

by

Sin

D

Cos4

1 (1)

where

“𝛽” is the full width at half maximum (FWHM) of the peak measured in radians,

“𝐷” is average crystallite size, and

“𝜀” is average lattice strain. The obtained XRD plots and the values of crystallite size

and average strain are given in Table 3.

Page 16: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Graph 1: XRD plot obtained for the Raw cotton sample from

X-ray Diffractometer Software.

Page 17: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Graph 2: XRD plot obtained for the Bleached cotton sample from

X-ray Diffractometer Software.

Page 18: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Graph 3: XRD plot obtained for the Irradiated Raw-10 cotton sample from

X-ray Diffractometer Software.

Page 19: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Graph 4: XRD plot obtained for the Irradiated Bleached-10 cotton sample from

X-ray Diffractometer Software.

Page 20: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Graph 5: XRD-Plots Obtained After Peak-Fit Method Smoothening for Raw and

Raw-10 Cotton Samples.

Page 21: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Graph 6: XRD plots obtained for Bleached and Bleached-10 cotton samples.

Page 22: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Graph 7: XRD plots obtained for the Raw and microwave irradiated Raw cotton

samples (Graphs are for arbitrary Scale obtained from origin ).

Page 23: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Graph 8: XRD plots obtained for the microwave irradiated Bleached cotton samples.

Page 24: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Table 3: Microstructural parameters obtained for the samples

Samples

Average

Crystallite Size in

Å

Average lattice strain in

%

Fig.8. Ringu MiniFlex II Desktop X-Ray Difractometer

Fig.9. Cotton Sample on Sample Holder of Ringu MiniFlex II Desktop X-Ray

Page 25: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Raw 60.68 1.47

After microwave irradiation for various time intervals

Raw 5 59.78 1.11

Raw 10 58 1.52

Raw 15 57.47 1.36

Raw 20 57.01 1.66

Samples chemically treated & Microwave treated

Bleached 61.76 1.62

Bleached 5 59.24 1.40

Bleached 10 58.80 1.93

Bleached 15 59.39 1.04

Bleached 20 60.87 1.58

Page 26: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

3.2. Results and Discussions of X-Ray Diffraction Studies:

It is seen from the XRD plots that there is no such significant changes in the

diffraction pattern obtained for the irradiated and unirradiated cotton samples at a

quick glance, but the changes in microstructure parameters are small in both irradiated

raw and bleached samples. There is overall increase in crystallite size values with

decrease in the microwave irradiation. This implies that there is scission of molecular

chains leading to more amorphous regions with microwave irradiation. There are

earlier reports on man-made fibres that this behavior is associated with decrease in

mechanical properties [3]. Bleached samples show a different behavior wherein the

crystallite size decreases initially and then increases. The reason being that a

continuous bleaching and radiation heat may change the polymer network leading to a

better ordering which leads to a slight increase in the crystallite size.

3.3. Conclusions:

We have quantified the changes in microstructural parameters in raw and

bleached cotton fibres using X-ray diffraction data. Further it is also observed that

there a gradual decrease in the values of crystallite size with increase in the dosage of

microwave radiation for raw cotton fibres. On the contrary, bleaching has a reverse

effect. All these changes are computed by considering the standard deviations

involved in the method.

Page 27: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

4. Studies on Physical, Mechanical & Dyeing Properties

4.1. Effect of Microwave Radiation on structure of fibres -

Microscopic Examination:

The longitudinal view of raw, bleached and micro- wave irradiated fibres were

observed using microscope Carl Zeis Axiostar Plus using 100 magnification.

The longitudinal views of raw and microwave irradiated fibres are presented in

fig 1, within the constraints of the experiment. The photographs were taken with the

available magnification (100). It may be observed from fig that the raw fibres show a

near cylindrical shape with minimum convolutions or twists. However the treated

fibres show bulging and open structure with clear convolutions and twisted

configuration . This is due to the effect of heat on the structure of fibres, increasing the

size of crystals leading to bulging of fibres.

Fig.10. Microscope Carl Zeis Axiostar Plus

Page 28: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Raw

Raw-15

Raw-10

Bleach

Bleach-5 Bleach-10 Bleach-15

Raw-10

Fig.11. Longitudinal Microscopic views of cotton fibres, using Microscope

CarlZeis Axiostar Plus using 100 magnification

Page 29: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

4.2. Moisture Regain:

Moisture Regain is the percentage of the mass of water which exists in the fibre

measured using the regulated method to the dry mass of the measured material.

Moisture Regain was measured directly by Using Instrument Humy Tester

Moisture Meter, Dried Cotton Fibres were exposed to atmosphere maintained at a 65

% RH by using Room Humidifier for 1 hour . Then the cotton samples were tested

with Humy tester.

The values obtained for of Moisture regain for Raw, Bleached and Microwave treated

cotton fibres are shown in Table 4.

Table 4: Moisture Regain of Raw & Bleached Cotton Fibres

Fig.12. Humidifier Fig.13. Humy Tester

Page 30: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Cotton Sample Moisture

Regain Cotton Sample

Moisture

Regain

Raw 7.5 Bleached 9.3

Raw-5 7.45 Bleached -5 9.26

Raw-10 7.41 Bleached -10 9.2

Raw-15 7.37 Bleached -15 9.14

Raw-20 7.31 Bleached -20 9.13

Results and Discussions:

Moisture Regain of Bleached cotton fibres shows an appreciable increase

compared to Raw Cotton Fibres. Moisture Regain for irradiated Raw and bleached

cotton fibres show a very small decrease which can be treated as negligible.

4.3. Mechanical Properties:

Tenacity, Breaking Elongation and Fineness Studies

Tenacity is the strength of the fibre. Stelometer was used to determine the

Bundle strength of fibres with 3 mm gauge length and CRL type loading. Percentage

breaking Elongation was also determined directly by Stelometer. Tenacity of the

fibres was calculated by using formula

G /Tex mg)in fibers of(Weight

10)×1.5×kgin load (Breaking =Tenacity

Fibre fineness is a weight of one-inch fibre. ( Linear Density) It is measured

in µg/inch. Fineness of the fibres was obtained by using Statex Fibre Fineness

Tester.

Page 31: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

The Tenacity, Breaking elongation percentage and Fineness values of raw and

irradiated cotton fibres are presented in Table 5.

Fig.16. Dye Bath

Fig.14. Stelometer Fig.15. Statex Fibre Fineness

Tester

Page 32: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

Table 5: Tenacity,%Breaking Elongation and Fineness for Raw, Microwave

treated Raw, Bleached and Microwave treated Bleached Cotton Fibres.

Cotton

Fibre

Tenacity

gm/Tex

% Breaking

Elangation

Finess

µg/inch

Raw 22.27 20 2.75

Raw -5 21.645 19 2.83

Raw-10 20.895 18.5 2.9

Raw-15 19.193 17.5 2.93

Raw-20 18.75 16.5 2.95

Bleach 23.4 19.5 3.25

Bleach-5 21.874 18 3.31

Bleach-10 23.57 17.5 3.36

Bleach-15 24.41 17 3.37

Bleach-20 20.85 16.5 3.2

Results and Discussions of Mechanical Properties:

It is observed that the tenacity of fibres exhibits a decreasing trend for raw

fibres to treated fibres. Elongation also follows the same trend. It shows a decrease for

treated fibres. This is due to scissoring of the chain molecules in the crystalline

regions leading to breaking of hydrogen bonds. Similar trend is also observed for

bleached fibres. Interestingly, the fineness of fibres shows an increasing trend both for

raw and bleached fibres.

Page 33: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

4.4. Dyeing Properties

4.4.1. Dyeing of fibres:

Bleached and Microwave exposed bleached cotton fibres for different time

intervals of 10, 15 & 20 min of known weight were taken in different dyeing baths

(Paramount Pvt Ltd). These fibres were dyed using a direct dye. Direct Dyes are

chemically Sodium salts of sulphonic acid. The dye bath was prepared using direct

dye of 3% shade, Sodium Carbonate of 3gm/l, with sample to liquid (water) ratio of

1:40. The fibres of known weight were put into dye baths at room temperature. The

temperature was gradually increased to 95o. Common Salt (40gm/l) was added in 3

equal installments as an exhausting agent. Dyeing was continued at this temperature

for 90min. After dyeing the fibre was washed with hot water and dried.

4.4.2. Dye Exhaustion percentage Studies:

Exhaustion % represents the amount of dye transfer from dye bath to fibre

(textile) material after dyeing. Absorption and Transmittance Percentage values of dye

liquid samples were determined using Elico double beam UV-VIS spectrophotometer

instrument and Elico Spectra treats double beam UV-VIS software. Dye exhaustion

was calculated by using formula,

100.×Af)/Ai-(Ai=E%

Where Ai=Initial absorbance Value before dyeing and

Af =Absorbance value after dying.

The dye exhaustion percentage values are presented in Table 6. It may be

observed that the exhaustion % and transmittance% of dye increases after the

microwave treatment.

Page 34: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

TABLE 6: Exhaustion % and transmittance %

Dye liquids after

Process Exhaustion% Transmittance %

Without Radiation 69.98 10.3

Dye-10min 70.16 10.5

Dye-15min 72.53 11.4

Dye-20min 76.74 15.4

4.4.3. K/S Studies:

K/S values represents color strength values of dyed sample.The dyed samples

were compared with undyed (standard bleached) cotton fibres for the spectral values

K/S, (CIE 2000) using Minolta 3301d Spectrophotometer with JAYPAK 4808

software in D65 daylight. This software is designed to find K/S values using the

formula

2R R)-(1

= K/S2

Where, K-represents absorption Co-efficient,

S-Scattering Co-efficient R-Reflectance value.

Fig.17. Spectro Photometer Fig.18. Elico double beam UV-VIS

spectrophotometer Dye Bath

Page 35: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

TABLE 7: Effect of Microwave radiations on K/S values obtained for the dyed

samples.

Cotton Fibre K/S

(Colour Strength)

Bleach (Std) 0.200

Dyed fibre

(without Radiation) 9.846

Dyed-10 9.942

Dyed-15 10.814

Dyed-20 11.807

The K/S values which represent the actual dye uptake by the fibres are

presented in Table. It may be observed that K/S values the of dye increases after the

microwave treatment. Untreated dyed fibre shows a value of 9.846 and the values

increase gradually for a treated fibre with increase in irradiation. A gradual increase in

dye uptake is observed after irradiation. This may be due to a reduction in crystallinity

and increase of amorphous content of fibres after heating treatments.

Page 36: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

CONCLUSIONS

The Raw and Bleached DCH-32 Cotton fibres were exposed to Microwave

radiations at different time intervals.

By using XRD data crystallite size and lattice strain were calculated. Raw

cotton fibres showed a gradual decrease in crystallite size with increase in the dosage

of Microwave radiations. On the contrary in case of Bleached cotton fibres crystallite

size has increased but again it shows variations. The reason being that bleaching and

radiation heat may change the polymer network leading to a better ordering which

leads to a slight increase in the crystallite size.

The Microstructural longitudinal view of Microwave treated cotton fibres

shows bulging and open structure with clear convolutions and twisted configuration.

This is due to the effect of heat on the structure of fibres, increasing the size of

crystals leading to bulging of fibres.

Moisture Regain of Bleached cotton fibres shows an appreciable increase

compared to Raw Cotton Fibres. Moisture Regain for irradiated Raw and bleached

cotton fibres show a very small decrease which can be treated as negligible.

The mechanical properties such as tenacity and breaking elongation reduce due

to breaking of hydrogen bonds and reduction in crystallinity and orientation.

The dye exhaustion and dye uptake (K/S values) indicates in increasing trend.

This result is helpful in dyeing of fibres with better results in textile industry.

Page 37: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

REFERENCES

1. C L Brubaker, A H Paterson, J F Wendel, “Comparative genetic mapping of allotetraploid

cotton and its diploid progenitors” Genome, 42, 2, 184-203, 1999.

2. S. Divakara, A. R. Niranjana, R. Somashekar "Computation of stacking and twin faults

in varieties of cotton fibres using whole powder pattern fitting technique" Cellulose,

16, 6, 1187-1200, 2009.

3. Youngchul Lee and Roger S. Porter "Crystallization of poly(etheretherketone) (PEEK) in

carbon fibre composites" Polymer Engineering and Science, 26, 9, 633-639, 1986.

4. A. R. Niranjana, S. Divakara, R. Somashekar, "Characterization of field grown cotton

fibres using whole powder pattern fitting method" Indian Journal of Fibre & Textile

Research, 36, 9- 17, 2011.

5. S.Paramasivam &A.R. Nagaraj "Effect of Microwave Radiation on Cotton and Rayon

Fabric" fibre2fashion june 06 2012

6. Nkemaja Dydimus Efeze, K.Murugesh Babu, N Jegna Ebenzerand Y.

Vrushabhendrappa. Textile Asia, 43, 11, 16-19, (2012)..

7. A. R. Niranjana, S. Divakara, R. Somashekar, Indian Journal of Fibre & Textile Research,

36, 9-17, (2011

8. Thejas Gopal Krishne Urs, Mahadevaiah Dasaiah and Rudrappa Somashekar, “Studies on

Structural and Conducting Properties of Goethite Nanoparticles Doped HPMC Polymer

Films”. Journal of Polymers, 2014, Article ID 201464, dx.doi.org/10.1155/2014/201464

Page 38: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

With Prof. K. Murugeshbabu, Chairman, Dept of Textile Technology at BIET,

Davangere

With Prof. R. Somashekar, Chairman, Dept. of studies in Physics & Prof. Umesh at

University of Mysore

Page 39: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor
Page 40: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor
Page 41: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor
Page 42: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor
Page 43: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor
Page 44: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor
Page 45: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor
Page 46: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor
Page 47: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor
Page 48: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor
Page 49: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor

At X-Ray Diffraction Laboratory & With Final BSC students at Dept. of Studies in Physics, Mysore University, Manasagangotri, Mysore.

Page 50: BAPUJI EDUCATIONAL ASSOCIATION ( R ) DAVANGERE of Treated and... · bapuji educational association ( r ) davangere d. r. m science college, davangere-577004 a report on ugc minor