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i Fabrication and Enhancement of Plasma Treated Cotton, Tencel Cotton and Modal Cotton with Antibacterial and Mosquito Repellent Finish By R.Prabha A Thesis Submitted to the Avinashilingam Institute for Home Science and Higher Education for Women Coimbatore – 641 043 In Partial Fulfilment of the Requirements for the Degree of Doctor of Philosophy in Textiles and Clothing December 2013

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Page 1: Final Revised thesis as on 1.3.15 front materialsshodhganga.inflibnet.ac.in/bitstream/10603/74022/8/prabha_intro.pdf · Doctor of Philosophy in Textiles and Clothing December 2013

i

Fabrication and Enhancement of Plasma Treated Cotton, Tencel Cotton and Modal Cotton with Antibacterial and

Mosquito Repellent Finish

By

R.Prabha

A Thesis Submitted to the

Avinashilingam Institute for Home Science and Higher Education for Women

Coimbatore – 641 043

In Partial Fulfilment of the Requirements for the Degree of

Doctor of Philosophy in Textiles and Clothing

December 2013

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ACKNOWLEDGEMENT If you realise that everyone is an individual with his own unique part to play than the power of tolerance is easy to develop.

- Sri Saibaba.

The investigator raises her humble heart in adoration to her Parents and God for showering their blessings to execute this research work successfully.

The scholar conveys her reverential gratitude to Late Dr.T.S.Avinashilingam, Founder, President and First Chancellor of Avinashilingam Institute for Home Science and Higher Education for Women – University, Coimbatore, for providing the heaven of learning along with his heavenly boon. She also owes her sincere gratitude to Late Dr. Rajammal P.Devadas, Former Chancellor, Avinashilingam Institute for Home Science and Higher Education for Women – University, Coimbatore. The investigator records her sincere thanks to Dr.T.S.K.Meenakshi Sundaram, M.A., M.Phil., Ph.D., Chancellor, Avinashilingam Institute for Home Science and Higher Education for Women – University, Coimbatore, for providing the infrastructural facilities for the conduct of the study.

The investigator is indebted to Dr.Sheela Ramachandran, M.Sc., P.G.Dip., Ph.D., Vice-Chancellor, Avinashilingam Institute for Home Science and Higher Education for Women – University, Coimbatore, for providing all the amenities required for the conduct of the study. The investigator records her gratitude to Dr.Gowri Ramakrishnan, M.Sc., M.Phil., Ph.D., Registrar, Avinashilingam Institute for Home Science and Higher Education for Women – University, Coimbatore, for providing all the help for the smooth conduct of the study.

The investigator likes to express sincere gratitude to Dr.U.K.Lakshmi, M.Sc., Dip.Ed., M.Phil., Ph.D., Dean, Faculty of Home Science for her motivation and support for this study. The investigator owes her heartfelt thanks to Dr.G.P.Jeyanthi, M.Sc.,

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M.Phil., Ph.D., Controller of Examinations, Avinashilingam Institute for Home Science and Higher Education for Women – University, Coimbatore, for her consistant help and support at all times of need. The researcher utters her heartfelt gratitude to Dr.K.Thangamani, M.Sc., Dip. Ed., M.Phil., Ph.D., Former Dean, Faculty of Home Science and Dr.P.Santhana Krishnan, Ph.D., Director, Research and Consultancy, Avinashilingam Institute for Home Science and Higher Education for Women – University, Coimbatore, for their constant help and support at all times of need.

The investigator owes her heartfelt thanks and deep sense of gratitude to Dr.N.Vasugi Raaja, M.Sc., M.Phil., Ph.D., Professor and Head, Department of Textiles and Clothing, Avinashilingam Institute for Home Science and Higher Education for Women – University, Coimbatore, for all her help, exemplary guidance and encouragement throughout this research work. Her guidance, encouragement and dedication have helped to shape up this thesis, it is privilege to work with her. Apart from the efforts of myself, the success of my research depends largely on the encouragement and guidelines of my guide.

The investigator wishes to record her heartful thanks to Dr.G.Krishna Bai, Former Dean, Faculty of Home Science and Professor and Head, Department of Textiles and Clothing, Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore, for her timely suggestions rendered for this study.

The investigator owes her special gratefulness to Dr.Saroja Prabakaran, M.A., Dip.Ed., Ph.D., Former Vice Chancellor for her encouragement.

The investigator records her thanks to Karunya Deemed University, Coimbatore, and RND Bio Soft, Coimbatore for testing the samples. The investigator is thankful to the librarian, Avinashilingam Institute for Home Science and Higher Education for Women, and South Indian Textile Research Association (SITRA), for the permission to use their library facilities.

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The investigator expresses her thanks to all the faculty members of the Department of Textiles and Clothing, Avinashilingam Institute for Home Science and Higher Education for Women – University, Coimbatore, for their tremendous support and help.

The investigator extend her heartful wishes to Mrs.D.Shobha Pai and Mrs.D.Sujatha Pai, Fast Forward her their excellent preparationof the research work.

The investigator expresses her thanks to her son Master Harikrishnan, Husband T. Sambamurthy, Brother, Sisters, Father in law, Mother in law, Brother in laws and Sister in laws. The researcher would like to thank all those who have directly or indirectly helped in the research work reported herein.

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LIST OF CONTENTS CHAPTER TITLE PAGE NO.

LIST OF TABLES xv

LIST OF FIGURES xvii

LIST OF PLATES xix

LIST OF APPENDICES xx

I INTRODUCTION 1

II REVIEW OF LITERATURE 11

2.1 Cotton Yarn 13

2.1.1 History of Cotton 14

2.1.2 Properties of Cotton 15

2.1.3 Uses of Cotton 16

2.2 Tencel Yarn 18

2.2.1 History of Tencel 19

2.2.2 Properties of Tencel 19

2.2.3 Uses of Tencel 21

2.3 Modal Yarn 22

2.3.1 History of Modal 22

2.3.2 Properties of Modal 23

2.3.3 Uses of Modal 24

2.4 Weaving 25

2.4.1 Classification of Weaving 26

2.4.2 Plain Weave 27

2.4.3 Mixtures 28

2.5 Finishing 28

2.5.1 Classification of Finishing 30

2.5.2 Scouring 31

2.5.3 Bleaching 31

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CHAPTER TITLE PAGE NO. 2.5.4 Functional Finishes 32 2.6 Plasma Application 33 2.6.1 Effect of Plasma on Fibres and

Polymers 35

2.6.2 Types of Plasma 35 2.6.3 Principles of Plasma 36 2.6.4 Classification and Application of

Plasma 36

2.6.5 Characteristics of Plasma Application 37 2.6.6 Advantages of Plasma Application 38 2.7 Microorganisms 40 2.7.1 Effect of Microbes on Textiles and

Humans 42

2.7.2 Effect of Mosquitoes 43 2.8 Antimicrobial Finish 43 2.8.1 Types of Antibacterial Finish 46 2.8.2 Properties of Antibacterial Finish 46 2.8.3 Requirements of Antibacterial Finish 47 2.8.4 Benefits of Antibacterial Finish 48 2.9 Mosquito Repellent Finish 50 2.9.1 Types of Mosquito Repellent 50 2.9.2 Requirements for Mosquito Repellent

Finish 51

2.9.3 Chemical Repellent 51 2.10 Natural Source 52 2.10.1 Guava Leaves (Psidium guajava) 54 2.10.2 Prickly Chaff Flower (Achyranthes

aspera) 56

2.10.3 Keelanelli (Phyllanthus niruri L.) 58 2.10.4 Vetiver roots (Vetiveria zizanioides (L.)

Nash)

58

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CHAPTER TITLE PAGE NO.

2.11 Phytochemical Analysis 59

2.11.1 FT-IR 59

2.11.2 Application of IR-Spectroscopy 60

2.11.3 Use of Infrared Spectroscopy 60

2.11.4 Scanning Electron Microscopy 61

2.11.5 Scanning Electron Microscopy (SEM) of the Finished Fabric

61

III EXPERIMENTAL PROCEDURE 63

3.1 Conduct of Survey 67

3.1.1 Selection of Area and Sample 67

3.1.2 Selection of the Tool 68

3.1.3 Pre-Testing of Interview Schedule 68

3.1.4 Conduct of Surveys 68

3.1.4.1 Market Survey 68

3.1.4.2 Consumer Survey 69

3.1.5 Final Conduct of Survey 69

3.1.6 Consolidation and Analysis of Data 69

3.2 Selection of Yarn 70

3.3 Fabric Formation 71

3.4 Pre-treatment of Fabrics 71

3.4.1 Scouring 73

3.4.2 Bleaching 73

3.5 Plasma Treatment 74

3.5.1 Selection of Gas 74

3.5.2 Parameters of Plasma Application 75

3.5.3 Application Method 77

3.6 Pilot Study 79

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CHAPTER TITLE PAGE NO.

3.7 Selection of Finishes 79

3.8 Selection of Herbs 79

3.8.1 Collection and Storage of Natural Herbs

79

3.9 Selection of Extraction Procedure 80

3.9.1 Solvent Extraction of Herbs 80

3.10 Phytochemical Analysis 83

3.10.1 Phytochemical Screening of the Herbal Extract

83

3.10.1.a. Identification of Alkaloids 83

3.10.1.b. Dragendroffs Test 83

3.10.1.c. Wagner’s Test 83

3.10.1.d. Identification of Flavanoids 83

3.10.1.e. Shinoda Tests 84

3.10.1.f. Decolorization Test 84

3.10.1.g. Ammonia Test 84

3.10.1.h. Identification of Terpenoids 84

3.10.2 Spectroscopic Study – FT-IR Analysis 85

3.11 Optimization Procedure 86

3.11.1 Optimization Parameters for Finishing 86

3.11.2 Method of Finishing 87

3.11.3 Padding Mangle Method 87

3.12 Evaluation of Fabrics 90

3.12.1 Physical Properties 90

3.12.1.a. Fabric Weight – ASTM D 3776-96

90

3.12.1.b. Fabric Thickness – ASTM D 3883-2004

91

3.12.1.c. Fabric Count – ASTM D 1059-01

91

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CHAPTER TITLE PAGE NO.

3.12.2 Mechanical Properties 92

3.12.2.a. Fabric Tensile Strength – ASTM D 5034

92

3.12.2.b. Fabric Elongation – ASTM D 5034

93

3.12.2.c. Fabric Abrasion Resistance – ASTM D 4158

93

3.12.3 Comfort Properties 94

3.12.3.a. Fabric Stiffness – BS 3356 – 1990

94

3.12.3.b. Fabric Crease Recovery – ASTM D 1295

95

3.12.3.c. Fabric Air Permeability – ASTM D 737-04

95

3.12.4 Absorbency Properties – AATCC 79 : 2007

96

3.12.4.a. Drop Test 96

3.12.4.b. Sinking Test 98

3.12.4.c. Capillary Rise Test 98

3.12.5 Antibacterial Assessment Test (Qualitative Test)

98

3.12.5.a. Agar Diffusion Test 100

3.12.5.b. Parallel Streak Test 100

3.12.6 Antibacterial Assessment Test (Quantitative Test)

101

3.12.6.a. AATCC Test Method 100-2004

101

3.12.6.b. Wash Durability Testing – AATCC 124-1996

101

3.12.6.c. AATCC Test Method – 124-1996

103

3.12.7 Mosquito Repellency Test 104

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CHAPTER TITLE PAGE NO.

3.12.8 Testing of Mosquito Repellency 104

3.12.9 Mosquito Collection 104

3.12.10 Repellency Behavioural Test 104

3.13 Scanning Electron Microscopy Analysis 106

3.14 Wear Study 106

3.15 Statistical Analysis of the Test Results 107

3.16 Nomenclature 108

IV RESULTS AND DISCUSSION 109

4.1 Findings of the Survey 111

4.1.1 Market Survey 111

4.1.2 Consumer Survey 112

4.2 Evaluation of the Antibacterial Finished Fabrics 113

4.2.1 Physical Properties 113

4.2.1.a. Fabric Weight 113

4.2.1.b. Fabric Thickness 115

4.2.1.c. Fabric Count in Warp and Weft Direction

118

4.2.2 Mechanical Properties 120

4.2.2.a. Fabric Tensile Strength in Warp and Weft Direction

120

4.2.2.b. Fabric Elongation in Warp and Weft Direction

123

4.2.2.c. Abrasion Resistance 126

4.2.3 Comfort Properties 128

4.2.3.a. Fabric Stiffness in Warp and Weft Direction

128

4.2.3.b. Fabric Crease Recovery in Warp and Weft Direction

131

4.2.3.c. Fabric Air Permeability 134

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CHAPTER TITLE PAGE NO.

4.2.4 Absorbency Properties 136

4.2.4.a. Fabric Drop Test 136

4.2.4.b. Fabric Sinking Test 139

4.2.4.c. Fabric Capillary Rise Test 141

4.3 Evaluation of the Mosquito Repellency Finished Fabrics

143

4.3.1 Physical Properties 143

4.3.1.a. Fabric Thickness 143

4.3.2 Mechanical Properties 144

4.3.2.a. Fabric Tensile Strength in Warp and Weft Direction

144

4.3.2.b. Fabric Elongation in Warp and Weft Direction

146

4.3.2.c. Fabric Abrasion Resistance 149

4.3.3 Comfort Properties 150

4.3.3.a. Fabric Stiffness in Warp and Weft Direction

150

4.3.3.b. Fabric Crease Recovery in Warp and Weft Direction

152

4.3.3.c. Fabric Air Permeability 154

4.3.4 Absorbency Properties 156

4.3.4.a. Drop Test 156

4.3.4.b. Sinking Test 157

4.3.4.c. Capillary Rise Test 159

4.4 Evaluation of Functional Groups Using FT-IR Method

161

4.5 Phytochemical Analysis Findings 164

4.6 Scanning Electron Microscope Analysis 165

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CHAPTER TITLE PAGE NO.

4.7 Antibacterial Evaluation 165

4.7.1 Agar Well Diffusion Evaluation 165

4.7.2 Bacterial Reduction Test – AATCC 100 Method

171

4.8 Wash Durability Test 174

4.8.1 AATCC 100 – 2004 Method 174

4.9 Mosquito Repellency Evaluation 179

4.10 Findings of the Wear Study 181

V SUMMARY AND CONCLUSION 183

REFERENCES 198

APPENDICES 210

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LIST OF TABLES TABLE NO. TITLE PAGE NO.

I Types of Gas Plasma Applied and their Effects 38

II Details About the Parameters of Plasma Application

78

III Phytochemical Test Screening 85

IV Optimized Parameters 87

V Washing Machine Conditions 103

VI Nomenclature 108

VII Market Survey 111

VIII Consumer Survey 112

IX Fabric Weight 114

X Fabric Thickness 116

XI Fabric Count in Warp and Weft Direction 118

XII Fabric Tensile Strength in Warp and Weft Direction

121

XIII Fabric Elongation in Warp and Weft Direction 124

XIV Abrasion Resistance 127

XV Fabric Stifness in Warp and Weft Direction 129

XVI Fabric Crease Recovery in Warp and Weft Direction

132

XVII Fabric Air Permeability 135

XVIII Fabric Drop Test 137

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TABLE NO. TITLE PAGE NO.

XIX Fabric Sinking Test 139

XX Fabric Capillary Rise Test 141

XXI Fabric Thickness 143

XXII Fabric Tensile Strength in Warp and Weft Direction

145

XXIII Fabric Elongation in Warp and Weft Direction 147

XXIV Fabric Abrasion Resistance 149

XXV Fabric Stiffness in Warp and Weft Direction 151

XXVI Fabric Crease Recovery in Warp and Weft Directions

153

XXVII Air Permeability 155

XXVIII Drop Test 156

XXIX Sinking Test 158

XXX Capillary Rise Test 159

XXXI FT-IR Analysis 161

XXXII Antibacterial Activity of Herbal Extract by Agar Well Diffusion Method

169

XXXIII Antibacterial Activity of the Finished Fabric – AATCC 100 Test Method

171

XXXIV Assessment of Antibacterial Activity by AATCC 100 – 2004 After 5th and 10th Washes

174

XXXV Mosquito Repellency Efficiency of Finished Fabrics by Improved Excito Chamber Method

179

XXXVI Findings of the Wear Study on Arm Pads 181

XXXVII Findings of the Wear Study on Cushion Covers 182

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LIST OF FIGURES FIGURE NO. TITLE PAGE NO.

1 Experimental Design 66

2 Schematic Diagram of Plasma Reactor 76

3 Fabric Weight 115

4 Fabric Thickness 117

5 Fabric Count in Warp and Weft Direction 120

6 Fabric Tensile Strength in Warp and Weft Direction

123

7 Fabric Elongation in Warp and Weft Direction 126

8 Abrasion Resistance 128

9 Fabric Stiffness in Warp and Weft Direction 131

10 Fabric Crease Recovery in Warp and Weft Direction

134

11 Fabric Air Permeability 136

12 Fabric Drop Test 138

13 Fabric Sinking Test 140

14 Fabric Capillary Rise Test 142

15 Fabric Thickness 144

16 Fabric Tensile Strength in Warp and Weft Direction

146

17 Fabric Elongation in Warp and Weft Direction 148

18 Fabric Abrasion Resistance 150

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FIGURE NO. TITLE PAGE NO.

19 Fabric Stiffness in Warp and Weft Direction 152

20 Fabric Crease Recovery in Warp and Weft Direction

154

21 Fabric Air Permeability 156

22 Drop Test 157

23 Sinking Test 159

24 Capillary Rise Test 160

25 FT-IR Analysis – Guava Leaves (Psidium guajava)

162

26 FT-IR Analysis – Prickly Chaff Flower (Achyranthes aspera)

162

27 FT-IR Analysis – Keelanelli (Phyllanthus niruri) 163

28 FT-IR Analysis – Vetiver (Vetiveria zizanioides) 163

29 Antibacterial Activity of Herbal Extract by Agar Well Diffusion Method

169

30 Antibacterial Activity of the Finished Fabric – AATCC 100 Test Method

172

31 Assessment of Antibacterial Activity by AATCC 100 – 2004 After 5th and 10th Washes

175

32 Mosquito Repellency Efficiency of Finished Fabrics by Improved Excito Chamber Method

180

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LIST OF PLATES PLATE NO. TITLE PAGE NO.

1 Selection of Yarn 72

2 Plasma Chamber 76

3 Selection of Herbs 81

4 Extraction Method 82

5 Padding Mangle Machine 89

6 Fabric Evaluation 97

7 Absorbency Properties 99

8 Antibacterial Activity Test AATCC – 100 Method 102

9 Mosquito Repellency Testing Method 105

10 Scanning Electron Microscopic Study 166

11 Vetiver Root (Vetiveria zizanioides) and Keelanelli (Phyllanthus niruri) Herbal Finished and Plasma Treated Herbal Finished Cotton, Tencel Cotton and Modal Cotton Fabrics Morphological Study

168

12 Antibacterial Activity of Herbal Extract by Agar Well Diffusion Method E. coli and S. aureus

170

13 Antibacteiral Activity of Guava Leaves 173

14 Assessment of Antibacterial Activity by AATCC 100 – 2004 Test Method After Washing Against E. coli and S. aureus (100% Cotton)

176

15 Assessment of Antibacterial Activity by AATCC 100 – 2004 Test Method After Washing Against E. coli and S. aureus (50 : 50 Tencel : Cotton)

177

16 Assessment of Antibacterial Activity by AATCC 100 – 2004 Test Method After Washing Against E. coli and S. aureus (50 : 50 Modal : Cotton)

178

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LIST OF APPENDICES APPENDIX NO. TITLE PAGE NO.

I Interview Schedule to Elicit Information from the Market

210

II Interview Schedule to Elicit Information from the Cnsumer about Arm Pads

211

III Interview Schedule to Elicit Information from the Consumer Abut Cushion Covers

212

IV Samples 213

V Proforma Used for Wear Study Findings 214

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ABSTRACT

Recently textile industry is facing enormous challenges such as highly

competitive market, ever-changing customer demands, cost reduction, value addition

and strict environment rules. Growing awareness for health and hygiene among the

people has increased the demand for anti-bacterial and mosquito repellent textiles.

Hence, considering the above facts, the investigator selected plants to impart

anti-bacterial and mosquito repellent finish. Based upon the phytochemical analysis

four phases namely Guava leaves (Pisidium guajava), Prickly chaff flower

(Achyranthes aspera), Keelanelli (Phyllanthus niruri) and Vetiver (Vetiveria

zizanioides) were selected. For this study, plain woven fabrics were prepared using

blends of cotton, modal and tencel yarn, plasma was created using oxygen gas

which was applied to the prepared fabrics. Both the untreated and plasma treated

fabrics were finished using the extracted herbs by padding technique. The fabric

evaluation was carried out using the standard testing procedure to measure the

physical, mechanical, comfort and absorbency of the fabric samples. The surface

morphological features of herbal finished and plasma treated herbal finished fabric

were evaluated by using scanning electron microscope. The anti-bacterial efficacy of

the fabrics was determined by bacterial reduction – AATCC 100, Agar diffusion and

parallel streak methods. Mosquito repellency test was performed by Excito chamber

method. The prepared end produces (arm pad and cushion cover) were subjected to

wear study and wash durability study.

Results from the study show that plasma treatment enhances the antimicrobial

efficacy of the fabrics examined, as evident from the durability of plasma treated

fabrics after washing. For example, in the case of fabrics without plasma treatment

the antimicrobial capability lasted only up to 15 wash cycles whereas, with plasma

treatment it lasted up to 25 wash cycles. Additionally, functional capability like

mosquito repellency was also improved based on subjective wear trials. The finish

will be useful in the commercial market, as most of the casual and formal garments

possess cellulosic textiles to the maximum extent.

Key Words : Antibacterial, mosquito repellent, plasma, fabrics, herbs and fabric

properties.