3. EXPERIMENTAL PROCEDURE

Transcription

1 3. EXPERIMENTAL PROCEURE The experimental Procedure pertaining to the title A study on the effect of multifunctional finishes on blended denim fabrics is discussed under the following headings. PHASE1 3.1 Pilot study The experimental procedure consisted of 4 phases.the first phase consisted of pilot study which includes market survey, consumer survey, Pretreatment, selection of herbs, extraction process of herbs, finishing method analysis of antibacterial activity by ENISO 2645 and Optimized parameters. The second phase consisted of application of multifunctional finish on selected fabrics and evaluation of the finished fabrics. In the third phase the multifunctional herbal extract was converted into microcapsules and applied on the fabric by pad dry cure method and the finished fabric evaluated and in the fourth phase the three extracted herbs were nano encapsulated and applied on the fabric by pad dry cure method and the finished fabric was evaluated. 3.2 Conduct of Survey Selection of shops and the consumer Formulation of the interview schedules Collection of data and consolidation of the data 3.3 Pretreatment esizing 3.4 Selection of herbs 3.5 Extraction process of herbs rying of herbs Grinding process extraction Aqueous extraction 3.6 Method of finishing Preparation of fabric Finishing of fabric 3.7 Preliminary analysis of qualitative antibacterial activity by ENISO Analysis of three selected herbs Optimization of herbal combinations of the three selected herbs Standardization of finishing process PHASE Optimized parameters 3.1Selection of multifunctional finishes Application of multifunctional finishes by dip method on four selected fabrics Analysis of the antibacterial activity on finished samples 34

2 3.1.3 Analysis of the antifungal activity on finished samples Anti odor evaluation on finished fabric Application of mosquito repellent finish PHASE Application of herbal extracts adopting microencapsulation method Microencapsulation of fabric by ionic gelatin process Finishing of selected fabrics using pad dry cure method Evaluation of microencapsulated finished fabrics PHASE: Application of herbal extract by nanoencapsulation method Procedure of nanoencapsulation method Finishing of selected fabric by pad dry cure method 3.13 Wash durability test Evaluation of finished fabric Visual inspection Geometrical properties Fabric Count Fabric weight (ISO 381: 1977) Fabric Thickness (IS 772: 1975) Mechanical properties Tensile Strength (ASTM : 1995) Abrasion Resistance (ISO : 1999) Pilling Resistance (ASTM- 3512/25) Comfort properties rape Coefficient (%) (IS-8357/1977) Air Permeability Test (IS 1156: 1984) Crease Recovery angle (IS 4681: 1981) Stiffness to fabric (IS 649:1971) Water Repellency spray test (AATCC22) Absorption properties Water absorbency test (AATCC 79:27) Sinking test Wickability test 3.15 SEM analysis for the best sample 3.16 FTIR analysis for the best sample 3.17 Statistical analysis of the study 3.18 Nomenclatures 35

3 3.1 Pilot study Flow chart of Phase 1 Conduct of survey Market survey Consumer survey Selection of fabric (A) 68% Cotton & 32% Polyester (B) 68% Cotton & 32% Poly Lycra (C) 68% Cotton & 32% Core Spun Lycra () 1% Cotton Pretreatment (desizing) Optimization of Parameters for finishing Selected 2 herbs Solvent used for extraction Proportions for selected 3 herbs Conditions for finishing Best 3 herbs Water and 1 Combinations followed 5 conditions followed Optimized Parameters Ricinus Communis, Senna Auriculata & Euphorbia Hirta Ricinus communis (methanol), Senna Auriculata (methanol) and Euphorbia Hirta (aqueous) 36 1:3:2 1 Part of Ricinus communis, 3 Parts of Senna Auriculata and 2 Parts of Euphorbia Hirta Standard Conditions (2Kg cm 2 Pressure, 2m min rpm)

4 Phase 2 APPLICATION OF MULTIFUNCTIONAL FINISHES AN EVALUATION Special finishes (optimized Parameters) Anti Bacterial AATCC 1 Anti Fungal AATCC 3 Anti Odor Mosquito Repellency ip Method Evaluation for four category properties Visual Inspection Physical Mechanical Comfort Absorbency Selected Sample (1% cotton) 37

5 Phase 3 MICROENCAPSULATION OF SPECIAL FINISHES AN EVALUATION Microencapsulation Best sample (1% cotton) Anti Bacterial ENISO 2645 Anti Fungal AATCC 3 Anti Odor Mosquito Repellency Pad ry Cure Method Evaluation Before, after 1, 2 and 3 washes Visual Inspection Physical Mechanical Comfort Absorbency Scanning electron microscopy [SEM] Fourier Transform Infrared Spectroscopy [FTIR] 38

6 Phase 4 NANOENCAPSULATION OF SPECIAL FINISHES AN EVALUATION Nanoencapsulation Selected Sample (1% cotton) Anti Bacterial ENISO 2645 Anti Fungal AATCC 3 Pad ry Cure Method Evaluation Before, after 1, 2 and 3 washes Visual Inspection Physical Mechanical Comfort Absorbency Scanning electron microscopy [SEM] Fourier Transform Infrared Spectroscopy [FTIR] 39

7 Phase -1 In phase 1 the investigator conducted two surveys namely market survey and consumer survey as part of pilot study. 3.2 Conduct of survey Market survey and Consumer survey consisted of the following steps: Selection of the shops and the consumer The market survey was conducted in 5 prominent shops which are located in Coimbatore. Those who sold denim material and garments were selected on the basis of random sampling method. An interview schedule was prepared to find out the preference of denim material as the market and consumer survey will be useful for selection of fabric, blends and required finishes on the denim material for this study. Hundred teenage girls & boys were selected for consumer survey to gather information about the following details. The interview schedule was prepared to find out the awareness on the following aspects. The finishes such as antibacterial, antifungal, anti odor, and mosquito repellency finishes were expected by the consumer on denim fabric Formulation of the Interview Schedule The interview schedule formulated for market and consumer surveys were as follows. The market and consumer survey consisting this aspect, are in Appendix I and Appendix II. Schedule I consist the name of the interviewer, name of the shop, selection of fabric, type of denim blends, preference of denim material,preference of color, amount spent on denim material and the weave used. Schedule II consisted of the name of the consumer, reason for the selection of denim material, awareness of finishes applied on denim fabric, preference of finishes on denim material, identification of finishes, opinion about the price, awareness about the care labels and frequency of wear of the denim garment Collection of ata and Consolidation of the data Reddy (24), states that the collection of relevant numerical data is the first step in any statistical enquiry and also adds that reliability of the data is the pre-requisite for forming reliable conclusions. A good rapport was established and the purpose of the study was explained to select the special finishes for antibacterial, antifungal anti odor, and mosquito repellency finishes. The interview was conducted by the interviewer, who used both schedules and recorded the information. 4

8 Selection of material Based on the survey the following four samples were identified for the further study. enim material sample A-68%cotton+32% Polyester, sample B-68%cotton+32% Poly Lycra, sample C- 68%cotton+32% core spun Lycra and sample -1% cotton woven by twill weave -2/1 RHT, weight - 7 ounces, and color - carbon tan.twenty three meters of each sample were selected for the study. The sample named as A, B, C and. Among the Twenty three meters three meter of sample were kept aside as original, in the remaining twenty meters, six meters was used for finishing and testing by dip method and two meters each of the samples were allotted for 1 washes, 2 washes and 3 washes. Four meters each of the samples was used for microencapsulation finishing methods and four meters for nanoencapsulation finishing methods. These finished fabrics were evaluated by visual inspection, for physical, mechanical, comfort and absorbency properties, and for microencapsulation and nano encapsulation method, the SEM and FTIR test was carried out. Selection of finishes Another aspect required by the consumer from the survey were special finishes for comfortable wearing of denim fabric such as antibacterial, antifungal, anti odor and mosquito repellent finishes and was selected for this study. 3.3Pretreatment esizing esizing is a process employed to remove the sizing materials present in the gray cloth to make it suitable for further processing. Typical denim wet finishing includes desizing to soften the fabric, as pointed by Yoon (25).The following recipe was used for desizing the selected A, B, C and denim materials. Recipe enim material - 2 meters (each) M: L ratio - 1meter : 15 liters Sodium hydroxide - 4 grams Temperature C PH - 7 Time - 3 minutes The esizing was done using the above ingredients, in selected four samples A, B, C, & individually for pretreatment. stainless steel vessel was used, In this vessel, 15 liters of soft water was poured and 4 grams of sodium hydroxide was added and made it dissolved in water and 2 meters of denim material was immersed and boiled for 3 minutes at boiling temperature 41

9 the ph was maintained at 7and stirred continuously The material was removed from the vessel and washed thoroughly with soft water and desized material was dried. 3.4 Selection of herbs For this research pilot study was conducted by selecting 2 herbs. The selected herbs botanical names are mentioned as follows. Live and healthy herbal plant parts of Ricinus Communis (leaves and seeds), Abutilon indicum (leaves), Solanum surattense (Leaves), Coccinia grandis (Fruits and leaves), atura metel (leaves with fruits), Aloe Vera (flower and leaves), Cardio spermum halicacabum (Leaves), Cissus quandrangularis (whole plant), Albizia amara (Leaves), Leucas aspara (Leaves), Euphorbia hirta (mixture of stem, leaf and flower), Kathari flower,cereus janacars (whole plant),tribulus terrestris (Whole plant), Senna auriculata(leaves ),Passiflora foetida ( Stem, Leaf and flower )and Poolapoo were collected from different region in and around Coimbatore district which were authenticated by the Botanical survey of India. The plant parts were washed twice in freshwater to remove epiphytes and other extraneous matter from the plants. The above selected 2 herbs were used for the selected finishes such as antibacterial, antifungal, anti odor and mosquito repellency finishes. 3.5 Extraction process of herbs The separated herbal parts were shadow dried and powdered by using dry grinding machine. The herbal powders were stored in a dry container for further studies. The herbal products today symbolize safety in contrast to the synthetics that are regarded as unsafe to human and environment. Although herbs had been priced for their medicinal, flavorings and aromatic qualities for centuries, the parts of the plant used for medicinal purposes are leaves, root, stem, fruits, the complete aerial parts, the whole plant, barks (root and stem) and flowers. However, leaves were found most frequently used part referred by Sravanthi et al (21) and joshi et al (29).The above herbs were selected after thorough study from the related books. The extraction process was done in three stages, such as drying, grinding and extraction. Two types of extraction method were followed such as methanol and aqueous extraction was done for all the selected twenty herbs and the following procedure was followed rying of herbs The collected plants were dried at the room temperature in the open air.it cannot be stored without drying to avoid breakdown of important compounds and also it will be contaminated by microorganisms. The dried herbs were kept in a dark room so that the break down of important components by sunlight will be prevented. After drying, those selected portions of the plant to be used and other parts of the plants were separated from dirt and other extraneous matter manually. 42

10 3.5.2 Grinding process ry Grinding of the selected herbal portion was done in grinder mixers. After that, the powder was sieved with seiver to remove the dirt and unkind particles. The fine powder obtained was used for extraction. The extraction was done by two methods such as methanol and aqueous extraction extraction individually. The following recipe was used for the extraction of selected 2 herbs Recipe Herbal powder - 6grams - 8 ml Aqueous (distilled Water) - 2 ml Temperature - Room temperature Time for incubation - 24 hours Filter paper - Whatmann no.1 filter paper Procedure for methanol extraction The above selected recipe was used for extraction. Six grams of the herbal powder was mixed thoroughly with methanol and water and it was kept in airtight conical flask. The conical flask was incubated for 24 hours in the room temperature. The supernatant was filtered using a Whatmann no.1 filter paper and the filtrate was dried and the methanol was evaporated at room temperature. When exposed to the air. The filtrate was collected and kept in an air tight container for further study. The same method was used to collect filtrates of herbal powder of selected twenty herbal samples. This procedure was followed with the reference of the article written by Thilagavathi and Krishna Bala (27), and Sathianarayanan et al (21) Aqueous extraction The following recipe was used for the aqueous extraction of selected 2 herbs. Recipe Herbal powder - 6grams Aqueous (distilled water) - 1 ml Temperature - Room temperature Time for incubation - 24 hours Filter paper - Whatmann no.1 filter paper 43

11 Procedure for aqueous extraction Six grams of dried herbal powder was mixed in 1ml of water slowly and mixed thoroughly in an air tight conical flask by shaking the flask for thorough mixing of herbal powder. The powder was allowed to dissolve in the water homogenously. Then the extract solution was filtered with Whatmann no.1 filter paper. The sediment/filtrate extract was allowed to dry in the room temperature. The filtrate/extract was collected and kept in an air tight container for further study. The same procedure was followed for selected twenty herbs. 3.6 Method of finishing Three methods of finishing of the fabric was selected for this study ip method for A, B, C and Pad-dry-cure method with microencapsulation for 1% cotton and Pad-dry-cure method with Nanoencapsulation for 1% cotton The above three methods were followed to finish with the above methanol and aqueous extraction on the selected fabrics Preparation of fabric The desized 1% cotton and its blended denim material was cut in to 1 cm X 1 cm.this sample was sterilized with UV rays in a laminar air flow chamber for 3 minutes and this was kept in a sterile place for further study Finishing of fabric The following recipe was used to finish the four selected fabrics by dip method using the extracted herbs. Recipe enim Samples - 2.5cm ±.1cm diameter Solvent - The above extracted methanol and aqueous Solvents Time - 2 minutes Sterilization - UV rays by Laminar air flow chamber Temperature - room temperature For finishing the fabric by dip method, the desized sterile samples was cut with circular disc of diameter 2.5cm ±.1cm.The extracted solvent was added in a beaker.the denim samples were immersed in the solvent for twenty minutes and then the sample were removed from the solvent and dried in the air without washing. The finished denim samples were sterilized by UV rays in the laminar air flow chamber to avoid microbial growth on the surface of the fabric. The same procedure was followed for the aqueous extract method of finish also. The sterile finished fabric sample was kept in a sterile container. 44

12 3.7 Preliminary Analysis of Qualitative Antibacterial activity ENISO 2645 method. The finished samples (both methanol and aqueous) were qualitatively assessed for the antimicrobial activity. The following microbes were selected for this study according to the ENISO 2645 standard. Test organisms - Escherichia coli ATCC and - Staphylococcus aureus ATCC 6538 Preparation of Inoculums The lyophilized sample of the above two strains of bacteria were inoculated in to a sterile peptone broth in a conical flask. The two conical flasks containing the bacterial samples were incubated at 37 ºC for 24 hours. The inoculums were ready for bacterial culture. Preparation of culture medium The cultural medium used for the qualitative study the bacteriostasis nutrient agar was prepared using the following ingredients. Recipe Peptone -.5 grams Yeast extract -.3 grams Sodium chloride - 2 grams Agar agar grams istilled Water - 1 ml The culture medium was autoclaved at 12 ºC for 15 minutes at a pressure of 15 lb. The Agar- agar medium was transferred into sterile Petri plates and allowed to solidify. This product was thus called as nutrient agar. This was used as subtract for the growth of the selected bacteria. Procedure for qualitative antimicrobial inhibition The inoculum of the test bacterial sample in the conical flask was inoculated. The cotton swabs dipped in the inoculums were swabbed on the Nutrient Agar surface uniformly. The sterile fabric samples were immersed in the herbal extract for 3 minutes and dried in sterile condition. Then this was placed in the nutrient agar surface using a sterile spatula and forceps. After placing the samples all the Nutrient Agar Petri dishes were incubated at 37 ºC for 18 to 24 hours. After incubation the plates were examined for the zone of bacterial inhibition around the fabric samples. The size of the clear zone of bacterial growth inhibition around the finished samples was evaluated which was the inhibitory effect of the herbal extract. 45

13 The above Antimicrobial finished samples were analyzed by Qualitative and Quantative method. This method was followed with the reference of Erdem and Yurudu (28) for this study. TABLE 2 Analysis of herbs for antibacterial activity by ENISO 2645 Antibacterial activity Zone of Bacteriostasis (mm) S. Solvents used Herb used No. for extraction Escherichia coli Staphylococcus aureus A B C A B C 1 Ricinus Communis Leaves Aqueous methanol Ricinus Communis Seeds Aqueous 28 3 atura metel - Leaves + fruit Aqueous * * * 32 4 Aloe Vera Flower Aqueous * 5 Abutilon indicum Leaves Aqueous Solanum surattense Leaves Aqueous methanol * * * 7 Coccinia grandis Fruit Aqueous methanol 8 Coccinia grandis Leaves Aqueous methanol 9 Aloe Vera Leaves Aqueous 28 1 Cardiospermum halicacabum Leaves Aqueous Tribulus terrestris Whole plant Aqueous Senna auriculata Leaves Aqueous Cissus quandrangularis Whole plant Aqueous Aibizia amara Leaves Aqueous 15 Leucas aspara - Stem, Leaf and flower Aqueous * * * Euphorbia hirta - Stem, Leaf and flower Aqueous Passiflora foetida Stem, Leaf and flower Aqueous Kathari flower Aqueous * * * 19 Cereus janacaru Whole plant Aqueous Poolapoo-whole plant Aqueous * - No bacterial growth beneath the test fabric. 46

14 Plate 1 Antibacterial activity of Ricinus Communis Leaves Against Escherichia coli against Staphylococcus aureus Water (Aqueous) Plate 2 Antibacterial activity of Water extract Ricinus Communis Seeds, atura metel and Aloe Vera Flower Ricinus communis seeds Water (Aqueous) atura metal Aloe Vera 47

15 Plate 3 Antibacterial activity of Methano extract Ricinus Communis Seeds, atura metel and Aloe Vera Flower Ricinus Communis seeds - atura metal Aloe Vera Plate 4 Antibacterial activity of Water extract Ricinus Communis Seeds, atura metel and Aloe Vera Flower Sample Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) 48

16 Plate 5 Antibacterial activity of Abutilon indicum - Leaves Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) Plate 6 Antibacterial activity of Solanum surattense Leaves Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) 49

17 Plate 7 Antibacterial activity of Coccinia grandis - Fruit Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) Plate 8 Antibacterial activity of Coccinia grandis Leaves Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) 5

18 Plate 9 Antibacterial activity of Aloe vera Leaves Against Escherichia coli Against Staphylococcus aureus Water (Aqeous) Plate 1 Antibacterial activity of Cardiospermum halicacabum Leaves Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) 51

19 Plate 11 Antibacterial activity of Tribulus terrestris Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) Plate 12 Antibacterial activity of Senna aurriculata -Leaves Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) 52

20 Plate 13 Antibacterial activity of Cissus quandrangularis Whole plant Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) Plate 14 Antibacterial activity of Aibizia amara Leaves Against Escherichia Coli Against Staphylococcus aureus Water (Aqueous) 53

21 Plate 15 Antibacterial activity of Leucas aspara - Stem, Leaf and flower Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) Plate 16 Antibacterial activity of Euphorbia hirta - Stem, Leaf and flower Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) 54

22 Plate 17 Antibacterial activity of Passiflora foetida Stem, Leaf and flower Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) Plate 18 Antibacterial activity of Kathari flower Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) 55

23 Plate 19 Antibacterial activity of Cereus janacaru Whole plant Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) Plate 2 Antibacterial activity of Poolapoo Against Escherichia coli Against Staphylococcus aureus Water (Aqueous) 56

24 Table 2 and Plates 1-2 Show the analysis of herbs for antimicrobial activity for twenty selected herbs, From the pilot study it was concluded that Ricinus communis, Senna auriculata and Euphorbia hirta have more antibacterial activity on the selected denim fabrics.hence the investigator selected the above three herbs for this study. 3.8 Analysis of three selected herbs The following table shows the scientific Name, Parts used, Common Name (English),Common Name (Tamil) and of the three selected herbs and was chosen for further study. TABLE 3 Ricinus communis, Senna auriculata and Euphorbia hirta Common Name Common Name Scientific Name Parts used S. No (English) (Tamil) 1 Ricinus communis Leaves Castor oil plant Amanakku 2 Senna auriculata Leaves Ranawara Avaram 3 Euphorbia hirta Leaves, Stem and Flower Asthma weed Amman pacharisi The above table shows the best three herbs selected based on the zone of incubation, evaluated under ENISO 2645 test method after it was conducted with 2 medicinal herbs and photographs of the plants as shown in plate

25 PLATE 21 Ricinuess communis Seena Auriculate Euphorbia Hirta 58

26 3.8.1 Optimization of herbal combinations of the selected three herbs: ic extract of Ricinus communis, ic extract of Senna Auriculata and aqueous extract of Euphorbia Hirta, were taken in to different ratio and finished on four selected denim fabric. The antibacterial activities of finished fabric were measured by Qualitative method as ENISO Antimicrobial activity against Gram-positive bacteria (Staphylococcus aureus) and Gram-negative bacteria (Escherichia coli) was tested according to ENISO 2645 test method. The following Table 4 shows that Analysis of Antibacterial activity on selected herbal combinations by ENISO 2645 Table 4 Proportion of three herbs by Ricinus Communies: Senna auriculata: Euphorbia hirta and the activity of antibacterial Zone of Inhibition (mm) Combinations Sl. No Escherichia coli Staphylococcus aureus Ratio of herbs A B C A B C 1. 1:1: :2: :1:1 * * * 4. 1:1: :2:1 * :2:2 * :1: :1: :3: :2:3 23 * - No bacterial growth beneath the test fabric. 59

27 Plate 22 Results for 1 Combinations for Four selected enim fabrics Escherichia coli Staphylococcus aureus 1A, 1B, 1C, and 1-1 part of ricinus communies, 1 part of senna auriculata and 1 part of euphorbia hirta, 2A, 2B, 2C and 2-1 part of ricinus communies, 2 part of senna auriculata and 1 part of euphorbia hirta, 3A, 3B, 3Cand3-2 part of ricinus communies, 1 part of senna auriculata and 1 part of euphorbia hirta. 4A, 4B, 4Cand4-1 part of Ricinus Communies, 1 part of Senna auriculata and 2 part of Euphorbia hirta. 5A, 5B, 5Cand5-2part of Ricinus Communies, 2 part of Senna auriculata and 1 part of Euphorbia hirta. 6A, 6B, 6Cand 6-1 part of Ricinus Communies, 2 part of Senna auriculata and 2 part of Euphorbia hirta. 6

28 Escherichia coli Staphylococcus aureus 7A, 7B, 7Cand7-2 part of Ricinus Communies, 1 part of Senna auriculata and 2 part of Euphorbia hirta. 8A, 8A, 8B, 8C and8-3 part of Ricinus Communies, 1 part of Senna auriculata and 2 part of Euphorbia hirta. 9A, 9B, 9Cand9-1 part of Ricinus Communies, 3 part of Senna auriculata and 2 part of Euphorbia hirta. 1A, 1B, 1Cand1-1 part of Ricinus Communies, 2 part of Senna auriculata and 3 part of Euphorbia hirta 61

29 3.8.2 Standardization of finishing process In order to standardize the finishing conditions in the pad-dry-cure method, the padding mangle was run at different pressure conditions and at different rpm. These were finished on the fabric at various conditions by maintaining constant pressure, varying the rpm, by maintaining constant rpm and varying the pressure. The various finishing conditions selected were 1. 2-kgf/cm 2 pressure (2 m/min rpm), 2. 2-kgf/cm 2 pressure (3 m/min rpm), 3. 3-kgf/cm 2 pressure (2 m/min rpm), 4. 3-kgf/cm 2 pressure (3 m/min rpm) and 5. 4-kgf/cm 2 pressure (2 m/min rpm). The finished fabrics were evaluated for antibacterial activity and the best finishing condition was standardized. The following are the different pressure and conditions to standard the finishing process Analysis of Antibacterial activity for fabrics finished under various conditions by ENISO 2645 Table 5 Analysis of antibacterial activity by ENISO 2645 Conditions for Finishing Pressure (Kgf/cm 2 ) and rpm 2kgf/cm 2, 2m/min (1) 2kgf/cm 2, 3m/min (2) 3kgf/cm 2, 2m/min (3) 3kgf/cm 2, 3m/min (4) 4kgf/cm 2, 2m/min (5) Samples Zone of Bacteriostasis (mm) Escherichia coli Staphylococcus aureus A B C A B C A B3 28 C * 27 A4 * 26 B4 * 26 C A B5 24 C * - No bacterial growth beneath the test fabric. Plate 23 62

30 Analysis of Antibacterial activity by ENISO 2645 for the fabrics finished under five different conditions Against Escherichia coli Against Staphylococcus aureus A1-2kgf/cm 2, 2m/min, A2-2kgf/cm 2, 3m/min, A3-3kgf/cm 2, 2m/min, A4-3kgf/cm 2, 3m/min, A5-4kgf/cm 2, 2m/min and B1 2kgf/cm 2, 2m/min B2-2kgf/cm 2, 3m/min, B3-3kgf/cm 2, 2m/min, B4-3kgf/cm 2, 3m/min and B5-4kgf/cm 2, 2m/min, C1-2kgf/cm 2, 2m/min, and C2-2kgf/cm 2, 3m/min 63

31 C3-3kgf/cm 2, 2m/min, C4-3kgf/cm 2, 3m/min and C5-4kgf/cm 2, 2m/min 1-2kgf/cm 2, 2m/min, 2-2kgf/cm 2, 3m/min, 3-3kgf/cm 2, 2m/min, 4-3kgf/cm 2, 3m/min and 5-4kgf/cm 2, 2m/min 64

32 PHASE: Optimized parameters. After conduct of Pilot study, the following parameters were selected for three herbs such as ic extract of Ricinus communis, ic extract of Senna Auriculata and aqueous extract of Euphorbia Hirta, in the proportion of (1:3:2). This extract was applied on the fabric by Pad dry cure method. This equipment speed was studied and 2Kg cm 2 Pressure, 2m min rpm was selected. 3.1 Selection of multifunctional finishes The phase 2 consisted of application of multi functional finishes such as anti bacterial finish using ENISO 2645 standard method and anti fungal finish was applied by AATCC 3 standard method,anti odor, mosquito repellency finish was given by dip method. The evaluation was done after 1, 2, 3 washes. The fabric was evaluated by five categories of evaluation such as visual inspection, physical, mechanical, comfort and absorbency property test. The above evaluation was done to find out the impregnation of multifunctional finishes in selected fabrics. The evaluation was done by comparing with ENISO 2645 tests for the accurate value Application of multifunctional finishes on selected four fabrics The dip method was followed to impart multifunctional finishes on selected A, B, C and fabrics. Recipe esized enim Fabric - 6 meters (each) Herbal powder - 36 grams (1:3:2) - (6:18:12) Material liquor ratio - 6meters:6 liters Test organisms - Escherichia coli ATCC Staphylococcus aureus ATCC 6538 Culture medium used - Bacteriostasis sterile agar broth Cultures Temperature - 37 ºC Time - 18 to 24 hours Sterilization - UV rays by Laminar air flow Chamber for 3 minutes The four selected materials namely A, B, C and were treated with the herbal extract. The fabric sample of 2.5cm ±.1cm diameter was taken for the analysis. Both sides of the sample were surface sterilized with UV rays for 3 minutes. The sterile nutrient agar was dispensed in sterile Petri dishes and allowed to solidify. Peptone broth culture of the test organisms were used as inoculums. Using sterile cotton swabs the test organisms i.e. - Escherichia coli ATCC and staphylococcus aureus ATCC 6538 was swabbed over the 65

33 surface of nutrient agar plate. Sterile samples A, B, C and was placed over the swabbed agar surface by using sterile spatula and forceps. After placing the samples the plates were incubated at 37 ºC for 18 to 24 hours. After incubation the plates were examined for the zone of inhibition around the fabric sample. The size of the clear zone around the sample was to evaluate the inhibitory nature of the herbs Analysis of the Antibacterial activity on finished sample The following method AATCC 1 was followed to evaluate the antibacterial activity on the finished 4 fabrics.this method was more accurate to evaluate antibacterial activity. Recipe Procedure esized enim Fabric - 6 meters (each) Herbal powder - 36 grams (1:3:2) - (6 grams: 18grams:12 grams) Material liquor ratio - 6meters:6 liters Test Organism Used - Escherichia coli ATCC Staphylococcus aureus ATCC 6538 Initial inoculums - E. coli 2.7 X 1 9 cfu/ml S. aureus 2.6 X 1 9 cfu/ml Culture medium used - Bacteriostasis sterile agar broth Test specimens - 5. cm diameter Temperature - 37 ºC Time - 24 hours Sterilization - UV rays by laminar air flow Chamber for 3 minutes About five cm diameter of the finished fabric was taken.1 ml of Sterile AATCC broth was taken in 5 conical flasks. In the first flask the sterile AATCC broth was kept undisturbed as a control sample (with out finished sample), the second broth.1 ml inoculums of Escherichia coli ATCC11229 (gram negative) was added, in the third flask.1 ml of Staphylococcus aureusatcc6539 (gram positive) inoculums was added, in the fourth flask five cm diameter of the finished fabric was put in.1 ml of Escherichia coli ATCC11229 inoculums, In the fifth flask five cm diameter of finished fabric was added along with.1 ml inoculums of Staphylococcus aureusatcc6539. The above five flasks of one negative control, two positive control and two with samples were incubated at 37 ºC for 24 hours then this incubated sample was transferred to a mechanical shaker. In the AATCC broth the fabric was put in the positive control i.e. AATCC broth with out the fabric was taken as inoculums for growth in the nutrient agar plates with appropriate dilutions. 66

34 Preparation of culture dilution The negative control in the conical flask no1 should not be disturbed where as the positive control sample and the broth with samples were diluted with sterile distilled water. The dilution of 1:2 lakh microorganism with.1 ml inoculum was prepared by dilutions methods and it is inoculated into nutrient sterile agar plates. The plates were incubated at 37 ºC for 24 hours. After incubation the results were interpreted with the number of colony forming units (cfu) in the nutrient agar plates with the inoculums from the four samples. The below mentioned formula is used for interpretation R (%) = (B A) x 1/ B Where A is the number of bacteria colonies from finished specimen after inoculation over 24 hours contact period and B is the number of bacteria colonies from unfinished control specimen Analysis of the Antifungal activity on finished samples The following were the evaluation of antifungal activity on the finished fabrics which was compared with the American association of textile chemist and colorist 3 for the accurate value. Recipe esized enim Fabric - 6 meters (each) Herbal powder - 36 grams Material liquor ratio - 6meters:6 liters Test organisms - Aspergillus Niger Culture medium used - inoculums of 1.ml Test specimens - 2cm ±.1cm diameter Temperature - 28ºC Time - for seven days Sterilization - UV rays by Laminar flow chamber for 15 Minutes. Procedure Inoculums of 1.ml were evenly distributed over the surface of the nutrient agar. The fabric sample was pre wetted (not rubbed or squeezed) in water containing.5% of a non-ionic wetting agent (triton X- 1) and placed on the agar surface. The inoculums of.2 ml were distributed evenly over each plate by means of a sterile pipette. All the specimens were incubated at a temperature of 28ºC for seven days. At the end of the incubation period the percentage of the surface area of the disc covered with the growth of the fungus was reported by observing visually using microscope (4X) and interpreted as follows: No growth (If present, the size of the growth free zone in mm was reported) 67

35 Microscopic growth (visible only under the microscope) Macroscopic growth (visible to the naked eye) Anti odor evaluation on finished fabric The following was the evaluation of anti odor activity on the finished fabrics which was compared with the organoleptic evaluation of odor control for accurate value. Procedure The selected male panelists wore the control and finished socks daily during the test period. Each sock was worn on a specific foot. At the end of the stipulated period of time, panelists had to remove the socks in the lab, and seal it in a plastic bag, and collect other socks for the next day. Four judges were selected to evaluate the odor finish from the worn socks. This evaluation was done after 14 hours of wearing of socks. The rating scale was prepared to 1(1-Ideal, 9-Excellent, 8-Very Good, 7-Good, 6-Fairly Good, 5-Acceptable, 4-Fair, 3-Poorly Fair, 2-Poor, 1- Very Poor and Repulsive) and was given to the judges for evaluating the effect of odor finish in the socks Evaluation of Mosquito repellent finish: The following was the evaluation of mosquito repellent finish on the finished fabrics. Selection of Mosquitoes Anopheles mosquitoes were identified based on morphologic keys; they were collected during the evening hours. All mosquitoes were starved for four hours and then fed blood and sugar kept in a bowl, before commencement of the tests. escription of the chamber Two specially designed excito-repellency test chambers were used to evaluate the efficiency of repellency activity. The wooden outer chamber of excito-repellency testing device (Plate24) measured 34 cm 32 cm 32 cm and faced the front panel with a single escape portal. The box was composed of a rear door cover, an inner Plexiglas glass panel with a rubber latexsealed door, a Plexiglas holding frame, a screened inner chamber, an outer chamber, a front door, and an exit portal slot. The selected anopheles Mosquitoes were deprived of all nutrition and water for a minimum of 4 hours before exposure inside the chamber Then these mosquitoes were placed inside the excito chamber for mosquito repellency efficiency test. This was performed only during daylight hours and each test was replicated four times. Observations were taken at one-minute interval for 3 minutes. After each test was completed, the number of escaped mosquitoes and those remaining inside the chamber was recorded separately for each exposure chamber, external holding cage, and paired control chamber. Escaped mosquitoes and those remaining inside the chamber were attracted by food and water. 68

36 Plate 24 Excito chamber used for test the Mosquito repellency efficiency No.of Mosquito escaped No.of Mosquito dead Efficiency of Mosquito repellency (%) = 1 No.of Mosquito exposed PHASE 3 From the dip method it was concluded that 1% cotton denim material was more suitable for the other finishing methods because in this fabric the wash durability was more than in other fabric. Hence for micro encapsulation and nano encapsulation only 1% cotton denim was used for finishing Application of herbal extracts adopting micro encapsulation method. In phase 3 the herbal extraction was microencapsulated and applied on 1% cotton denim fabric() by pad dry cure method to get antibacterial, antifungal, anti odor and mosquito repellency finishes and this was evaluated after 1,2 and 3 washes. The evaluation was done by seven categories such as visual inspection, physical, mechanical, comfort, absorbency. A scanning electron microscopy and Fourier transform infrared spectroscopy test was carried out and it was applied on the selected fabric Micro encapsulation of fabric by ionic gelatin process Preparation of Microencapsules Micro encapsulation method was followed as said by Sathianarayanan et al (21).This procedure, adopted to prepare multifunctional finishes was encapsulated and applied on 4 selected fabrics. Encapsulation was a process of entrapping a tiny core material, typically a small solid particle or a liquid droplet or a gas bubble, inside a wall material. Generally, the wall 69

37 materials are natural or synthetic polymers, metal or inorganic oxides suitable for particular end application like insect repellent, antimicrobial etc,as pointed by Palanikkumaran et al (21).Micro encapsulation was the cost effective and long lasting method in storing volatile substances over a long period of time pointed by Ocepek et al (28). The microencapsules were applied on the fabric by pad dry cure method. Recipe enim Fabric - 4 meters Herbal powder (core) - 24 grams Material liquor ratio - 4:4 Sodium alginate (wall) - 3% Time - 2 hours Temperature - 45 C Solvent - Calcium chloride Procedure for Micro encapsulation Microcapsules containing extracts of herbal combinations 1 Part of Ricines Communis, 3 Parts of Euphorbia Hirta and 2 Parts of Senna Auriculata as core material and sodium alginate as the wall material was prepared. Ten grams of wall material was allowed to swell for half an hour by mixing with 1 ml of hot water. To this mixture 5 ml of hot water was added and stirred for 15 minutes maintaining the temperature between 4 C and 5 C. to this mixture, 1 ml of core material sodium alginate was added and this was transferred to a centrifuge and rated at 3-5 rpm speed for 15 minutes. This was sprayed into 2% of calcium chloride solution by means of a sprayer. The droplets were retained in calcium chloride collection bath for 15 minutes. In this bath the calcium ions diffused with the alginate solution, thereby hardening the matrix and forming a solid hydro gel system. The microcapsules were obtained by decantation and repeated washing with isopropyl alcohol followed by drying at 45 C for 12 hours. The microcapsules were then used for finishing on the selected fabrics with pad dry cure method Finishing of selected fabrics with pad dry cure method. The main challenge in the process of developing microcapsules with application in the textile industry was to produce a capsule with adequate mechanical strength to ensure the process of application to the textile. Additionally, the obtained microcapsules had to provide desired mechanism and release of encapsulated compounds, which had more stability and nontoxicity. Microencapsules can be applied to textiles by padding, coating, spraying or immersing without altering their feel or color. The investigator had followed pad dry cure method as stated by 7

38 Mulasavalagi (25). Citric acid was used as a binder to fix the finishing permanently on the fabric. Recipe enim fabric - 4 Meter (1% Cotton) Microcapsules - 2% Binder (Citric acid) - 8% Temperature - 55 C Time - 3 minutes The basic process was that the microencapsules were compounded at a certain ratio and padded on the fabric.the microencapsules were attached to the fabric with binder. By evaporating water during the drying process in a tenter, it allows only the required ingredients to combine with the fabric. ROLLER MANGLAR FABRIC FABRIC LOSS BATH Figure 1 pad dry cure process The Compounded solution consisted of 2% of the microencapsules with binder citric acid 8% and normal textile chemicals were added, such as softener, anti-static electricity agent and was kept in a bath. The fabric was dipped into the compounded solution using a roller. The fabric was sent through a padding mangle to squeeze the dipped chemicals out of the bath at the ratio of the pick up rate when the fabric was passed between the rollers. The heat dryer dried the fabric with heat for evaporating water and maintaining its width. The encapsulation worked inside the fabric, filling the spaces between the fibers with an ultra thin film of polymer creating a permanent barrier that was breathable, yet impermeable to both water and wind. 71

39 Evaluation of microencapsulated finished fabrics The selected multi-functional finishes such as,anti bacterial finish using ENISO 2645 standard method,anti fungal finish by AATCC 3 standard method, anti odor, mosquito repellency finish was done by micro encapsulation technique on selected 1% denim fabric by using pad dry cure method. The evaluation was done after finishing the sample and the wash durability test was conducted in three stages of 1, 2 and 3 washes. The finished fabric was evaluated and compared with the unwashed samples. The evaluation was done with five categories namely visual inspection, physical, mechanical, comfort and absorbency property test. A scanning electron microscope and Fourier transform infrared spectroscopy was used to find and evaluate the impregnation of micro encapsulation finishes in selected fabrics. PHASE: Application of herbal extract with Nanoencapsulation method In phase 4 the herbal extraction was nano encapsulated and applied on 1% cotton denim fabric () by pad dry cure method to get antibacterial and antifungal finish, and this was evaluated after 1, 2 and 3 washes. The evaluation was done using seven categories such as visual inspection, physical, mechanical, comfort, absorbency, A scanning electron microscopy and Fourier transform infrared spectroscopy test, and it was applied on the selected fabric for increasing the durability of the finishing on the fabric Procedure of Nanoencapsulation method Preparation of nanoencapsules The herbal extracts prepared were encapsulated using bovine albumin fraction as the wall material and the nanoparticles (herbs) as the core material. Recipe enim fabric - 4 meter (1% cotton) Herbal powder (core material) - 96 grams Material: Liquor ratio - 1:2 Bovine serum albumin (wall) - 2% W/V Binder (Citric acid) - 8% Temperature - 55 C Time - 3 minutes The herbal extract was enclosed by bovine serum albumin protein prepared by coacervation process followed by cross-linking with glutaraldehyde. After glutaraldehyde treatment, it was purified and passed through a rotary vacuum evaporator to remove the organic solvent. The sample was then centrifuged at 4 degree Celsius (1, rpm) and then suspended in.1m phosphate buffer and the ph was maintained at 7.4, then lyophilized with mannitol (2% w/v). 72

40 Procedure The herbal extract was incubated with the required protein i.e. Bovine albumen fraction solution (2% W/V) for an hour at room temperature. The ph of the solution was adjusted to 5.5 by adding 1molar HCL using digital ph meter. Then ethanol was added to the solution in the ratio 2:1 (V/V). The rate of ethanol addition was carefully controlled at 1 ml per minute. The coacervate so formed was hardened with 25% glutaraldehyde for 2 hours to allow cross-linking of protein. Organic solvents were then removed under reduced pressure by rotary vacuum evaporator and the resulting nanocapsules were purified by centrifugation at the speed of 1, rpm and the temperature was maintained at 4ºC. Pellets of nanocapsules thus obtained, were then suspended in phosphate buffer (ph -7.4;.1 M) and each sample was finally lyophilized with mannitol (2% W/V). The nanocapsules obtained were further dried by lyophilisation and were applied on the cotton fabric by exhaustion method using 8% citric acid as binder. The antibacterial activity of the nanocapsules finished fabric was evaluated by ENISO 2645 test method Finishing of selected fabric by pad dry cure method Recipe enim fabric - 4 Meter (1% Cotton) Nanocapsules - 2% Binder (Citric acid) - 8% Temperature - 55 C Time - 3 minutes The basic process was that the nanocapsules were compounded at a particular ratio and padded on the fabric.the nanocapsules were attached to the fabric with binder. By evaporating water during the drying process in a tenter, it allows only the required ingredients to combine with the fabric. The Compounded solution consisted of 2% of the nanocapsules with binder citric acid 8% and normal textile chemicals were added, such as softener and anti-static electricity agent and kept in a bath. The fabric was dipped into the compounded solution using a roller. The fabric was sent through a mangler to squeeze the dipped chemicals out of the bath at a certain ratio by the pick up rate when the fabric was passed between the rollers. The heat dryer dried the fabric with heat for evaporating water and maintaining its width. The encapsulation worked inside the fabric, filling the spaces between the fibers with an ultra thin film of polymer creating a permanent barrier that was breathable, yet impermeable to both water and wind. 73

41 3.13 Wash durability test The greatest influence was made by washing. uring the whole washing cycle, garments were affected by the entire complex of different factors such as a washing solution, abrasion, creasing, heat, various chemicals etc, says Juciene et al (26). The dip micro encapsulation and Nanoencapsulation finished fabrics were analyzed for wash durability by subjecting the samples to washing by industrial machines and testing. The washed fabrics were assessed by ENISO 2645 test methods Evaluation of finished fabric Visual inspection The visual inspection was conducted for multifunctional finished (dip, micro encapsulated and nano encapsulated) fabrics.this was done by a panel of juries containing 5 members, possessing textile knowledge. The juries evaluated the samples using the prepared rating scale for the visual inspection as given in (appendix-3) which included details regarding general appearance, color, luster and texture of the sample Geometrical properties Fabric Count Fabric count was measured using counting glass according to ASTM standard, point out as and Kothari (212). The fabric count was the number of warp and weft yarns per unit distance while the fabric was held without tension and free folds and wrinkles. The number of warp threads/inch was called ends/inch. The threads of weft were called picks and the number of weft threads per inch was called picks/inch. Therefore, a fabric may be described in terms of ends and picks pointed by Angappan and Gopalakrishnan (21). Use of counting glass (pick glass) The counting glass was a small magnifying glass in a stand over a square exactly one inch each way. The number of ends and picks per inch should be counted in five different places and the mean value is calculated and the test repeated for twenty eight samples Fabric weight (ISO 381: 1977) Fabric weight was measured according to ASTM Test Method say Sarkar (24). The specimen of known area was dissected into warp and weft threads over paper of a color suitable for showing up fragments of yarn from the fabric being tested. When the dissection of the specimen was completed, the non-fibrous matter from the two sets of threads was removed separately by a method described in ISO/TR59, taking care that no loss of fiber occurred during the process. The threads were and brought into equilibrium in the standard atmosphere for testing, from the dry side by exposing them freely to that atmosphere. The mass of the two sets of threads was determined separately to get an accuracy reset of.1%. 74

42 From the conditioned masses of warp and weft, free from added matter, and the known area of the specimens dissected, mass per unit area of warp, and weft of fabric was calculated, and each expressed in grams per square meter. The same procedure was repeated for five samples and the mean values were calculated and the test repeated for twenty eight samples Fabric Thickness (IS 772: 1975) The principle of measuring fabric thickness in B.S.2544:1954: states that essentially, the determination of the thickness of a compressible material such as a textile fabric consists of the precise measurement of the distance between two parallel plates as a pressure foot and the other as the anvil, says Jewel Raul (29). The pressure foot and the reference plate were cleaned. The pressure foot shaft was checked for free movement. With the pressure foot so loaded as to exert the appropriate specified pressure on the reference plate, the thickness gauge was set to zero. The pressure foot was raised and the sample was positioned without tension on the reference plate, such that no part of the area to be measured was near the selvedge. The area chosen for the test was ensured that it was free from creases. No attempt to flatten out any creases was made, as it was likely to affect the result. The pressure foot was gently lowered onto the sample; the gauge readings were noted down after 3 seconds. Similarly, the thickness was determined at five places on the sample chosen, containing different warp and weft threads and the test repeated for twenty eight samples Mechanical properties Tensile Strength (Kg) (ASTM : 1995) Akshay et al (211) states that the Tensile strength was measured according to ASTM 1682 Procedure. Fabric Tensile Strength (Kg) (ASTM : 1995) (plate 25) was used for the study. The specimen was mounted in the clamp jaws with the drawn parallel line adjacent to the side of the upper and lower front or top, jaws which were nearest to this edge, and with approximately the same length of fabric extending beyond the jaw at each end. The parallel line served as a guide to ensure that the same lengthwise yarns of woven fabrics were gripped in both clamps. For high-strength fabrics where the specimen could not be satisfactorily held in clamps, each specimen was placed around pins and between jaws, using jaw padding if necessary. The clamps were tightened to distribute the holding pressure along the clamping surface of the top (front) jaw. Clamps which were too tight would produce breaks at the front of the jaws; clamps which were too loose would cause slippage or breaks at the back of the jaws. 75

43 Elongation depended on the initial specimen length which was affected by any pre-tension applied in mounting the specimen in the testing machine. If measurement of specimen elongation was required, the specimen was mounted in the upper clamp of the machine and a uniform pretension applied, not to exceed.5% of the full-scale load to the bottom end of the specimen, before gripping it in the lower clamp. To achieve uniform and equal tension, an auxiliary clamp (6.3) was attached to the bottom of the specimen and at a point below the lower clamp. The specimen at the front inner edge of each jaw was marked to check for specimen slippage. When slippage occurred, the mark would move away from the jaw edge. The machine was operated and the specimen was broken. The breaking force and elongation was read if required, from the mechanism provided for such purpose. Warp and filling direction results were recorded separately. The same procedure was repeated for five samples and the mean value was calculated for twenty eight samples Abrasion Resistance (ISO : 1999) Abrasion tests were performed on a Martindale Abrasion Tester as referred by Ulku et al (23).Abrasion was just one aspect of wear and was the rubbing away of the component fibers and yarns of the fabric, notes Basu (26).The Abrasion Resistance (ISO : 1999) (plate-26) was used to measure the Abrasion Resistance of the fabric. The abrasion tester was started and continued without interruption, until the pre-selected number of rubs was reached. the specimen holder with the mounted specimen was carefully removed from the testing machine; and, without damaging or disturbing the threads, the whole area was examined for signs of breakdown. If no breakdown had yet been established, the holders were replaced in the machine, and the next test interval was started. This test and assessment sequence was continued, until a breakdown was observed. The specimen was inspected with the aid of a magnifying device. If the number of rubs exceeded 5, the test was interrupted every 5rubs, or earlier if required, in order to renew the abrading. In case where the interruption occurred before the completion of 5 rubs, the specimen holders with mounted test specimens were carefully removed from the testing machine, in order to avoid damage. The abrasion test was continued, until all specimens reach the specified end point/breakdown. The same procedure was repeated for five samples and the mean value was calculated for twenty eight samples. 76

44 Pilling Resistance ASTM- 3512/25 According to Gokarneshan et al (211), the pilling resistance of the samples was measured using ICI Pill box tester using IS: test method with standard abrading surface. This test method covered the resistance to the formation of pills and other related surface changes on textile fabrics. The Pilling tester ASTM- 3512/25 (plate -27) was used to measure the pilling resistance of the fabric. All tests were done in the standard atmosphere for testing textiles. Three specimens, all from the same sample, were placed and about 25 mg of 6-mm (.2-in.) denim fabric into the test chamber. The chamber was covered, and the timer set for a running time of 3 min. the motor was switched ON, the START button pushed, and the air flow started. uring the course of the run, each test chamber was checked at frequent intervals. If a specimen wedged around the impeller without tumbling or remained inert on the bottom or side of the chamber, the air was shut off, the machine stopped, the faceplate removed, and the specimen freed. Any hang-ups or other abnormal behavior of the specimens were recorded on the data sheet. When a specimen wedged around the impeller during arum, the test was stopped, the impeller blade was cleaned as directed, after each time run, each specimen was removed and the excess fiber that was not actually entangled in pills was cleaned away with the vacuum cleaner. The specimen was firmly grasped by a corner and all specimens were vacuumed in this manner. The test chamber was vacuumed.the shaft of the impeller was cleaned, using a sharp instrument, such as a pick needle to remove trapped detritus. For evaluation, each specimen was placed on the double-faced tape in the viewing cabinet. Using the viewing apparatus and options selected subjectively, the appearance of the fabric of each specimen was rated, using the following scale. 5- no pilling, 4-slight pilling, 3- moderate pilling, 2-severe pilling, 1-very severe pilling. The same procedure was repeated for five samples and the mean value was calculated for twenty eight samples Comfort properties rape Coefficient (%) (IS-8357/1977) According to BS-558/1973, it is defined as the percentage of the total area to an annular ring of fabric obtained by vertically projecting the shadow of the draped specimen, say Bhalerao (27). Fabric drape was the hanging property of the fabric and is inversely proportional to drape coefficient of the fabric, say Tyagi et al (211). The rape Coefficient [(%) (IS-8357/1977) (Plate -28)] was used to measure the drape of the fabric. rape is one of the subjective performance characteristics of a fabric that contributes to aesthetic appeal, says Indian standards, (1977). The drape tester was placed firmly on a level table. The light was switched on. The specimen holder was removed from the bayonet socket and a cut fabric specimen was placed between the plates. The stub of the 77

45 specimen holder assembly was held, and briskly moved up and down ten times, and tested on the table each time, for a moment. A square of ammonia process paper on the base of the instrument was placed flat. The stub of the specimen holder was inserted in the socket on the threaded bolt, pressed upwards and turned counter clockwise to lock the holder in position. Looking along the level of the base board, the height of the drooping edge of the drape specimen was adjusted, so that the lowermost edge was just above the paper without touching it. The setting knob of the timer was adjusted for the required time of exposure. At the end of the exposure time, the ammonia paper was removed, and placed in a developing box containing a few millimeters of strong ammonia solution. When the latent was developed, the paper was removed. The paper was conditioned to moisture equilibrium in standard atmosphere. The drape pattern was cut out with a pair of scissors and its mass determined in gram weight, exact to two decimal places. Mass per unit area of the paper was determined, by cutting a known area of the original paper and weighing. The specimen was reversed and the drape pattern obtained with the other surface upwards. The following formula was used to calculate the percentage of drape coefficient. rape co-efficient (F %) = W/w-a / A-a *1 Where, mass of drape pattern (gms) = w Mass/unit area of the paper= W Area of circle of 12.5 cm diameter = a Area of circle of 25 cm diameter = A rape was the ability of a fabric to fall under its own weight into wavy folds of different nature. Fabric drape can be evaluated objectively as well as subjectively. The same procedure was repeated for five samples and the mean value was calculated for twenty eight samples Air Permeability Test (IS 1156: 1984) The air permeability was defined as the volume of air in milliliters which was passed in one second through 1 smm2 of the fabric at a pressure difference of 1 mm head of water by Tugrul Ogulata (26). Air Permeability Test (IS 1156: 1984) was based on the measurement of the rate of flow of air through a given area of fabric by a given pressure drop across the fabric denotes Indian standard, 1985.A portion of the conditioned specimen was mounted between the clamp and the circular orifice with sufficient tension to eliminate wrinkles, if any and care taken to ensure that the fabric was not distorted. The suction fan or other means to force air through the fabric was started; the rate of the flow of air was adjusted till a pressure drop of one centimeter water across the fabric was indicated. The rate of air flow was noted in cm 3 /s. The test was repeated at different places. The same procedure was repeated for five samples and the mean value was calculated for twenty eight samples. 78

46 Crease Recovery angle (IS 4681: 1981) The test specimen was creased for a definite period of time at a known load and then allowed to recover or to regain its crease. The recovery was measured in terms of the extent of angle to which it had been recovered. Cloth crease recovery angle (degree) was denoted by Sujata and Mulasavalagi (25). Crease recovery is the property of the fabric to recover back to its original position after removal of certain load from the folded fabric says Tyagi (29). Crease recovery of fabrics by determining the angle of recovery after the removal of creasing force is referred in Indian standard (1981). The testing equipment was leveled with the help of leveling screws and the spirit level. Level the testing equipment with the help of leveling screws and spirit level. The specimen was folded end to end in half, with its edges gripped in a line with the help of tweezers, no more than 5 mm from the ends the folded specimen was placed on the plate of the loading device and load was applied gently without delay. The load was removed after 5 minutes. The removal of the load should be done in.5 seconds. Half of the specimens were folded face to face and the other half back to back. In order to mount, the one limb of the specimen was placed in the clamp of the instrument and the other held by the tweezers, in such a manner to ensure that there was hardly any disturbance. The specimen was thus held for at last one minute before the angle was measured. While the specimen was held by the clamps, adjustments were made such that the suspended limp of the specimen is always in a vertical position or horizontal position depending upon the type of instrument used. The reading of the crease recovery angle was taken after 5 minutes after the load was removed. The angle of recovery was measured for all the warp way and weft way specimens folded face to face and back to back in the same way. The same procedure was repeated for five samples and the mean value was calculated for twenty eight samples Stiffness to fabric (IS 649:1971) Method for determination of stiffness of fabrics as denoted by Indian standard, 1971 (plate-29).the tester was placed on a table or bench so that horizontal platform and inclined reference line were at eye level of the operator. The platform was adjusted, with the help of a spirit level so that it was horizontal. One of the specimens was placed on the platform with the scale on top of it lengthwise and the zero of scale coinciding with the leading edge of the specimen. The scale was held in the horizontal plane, the specimen was pushed, and the scale slowly and steadily moved, when the leading edge projected beyond the edge of the platform. An increasing part of the specimen would overhang and start bending under its own weight. If the specimen had a tendency to twist, a reference point was taken at the center of the leading edge. The specimen which twisted more than 45 degree was not measured. The length of the overhanging portion was noted from the 79

47 scale to the nearest millimeter. five readings from each specimen was taken, with each side up, first at one end and then at the other. Similarly, at least five test specimens for each warp way and weft way was tested. The weight per unit area of the fabric was determined, according to IS: I and expressed in terms of milligrams per square centimeter. Alternatively the weight per unit area could be determined by weight of all the warp way and weft way test specimens together, after completion of stiffness test. The same procedure was repeated for five samples and the mean value was calculated for twenty eight samples. According to Gnanavel and Ananthakrishnan (211), the pierce cantilever test was performed on the Shirley stiffness tester. Flexural rigidity of the fabric samples was calculated as per the ASTM using Shirley fabric stiffness tester, say Saravanan et al (211) Water Repellency spray test (AATCC22) According to Ghosh (211), the standard test method for the water repellency measurement of woven textile fabrics was used (SIST EN492). Water Repellency spray test (AATCC22) (plate -3) was used to test the fabrics. Before testing was carried out, the specimen should be conditioned for at least 24 hours in the standard atmosphere. Water sprayed against the taut surface of a test specimen under controlled conditions, produced a wetted pattern whose size depended on the relative repellency of the fabric. To carry out the test, test specimens were fastened securely in the metal hoop of the water repellency tester so that it represented a smooth wrinkle free surface and placed face up on the tester. The metal hoop was adjusted, so that the centre of the spray coincided with the centre of the metal hoop. Later, 25 ml of distilled water at normal temperature, was poured into the funnel and the whole quantity sprayed on the test specimen for a period of 25-3 sec. (AATCC standard). Then, the metal hoop was detached from the stand, and confirmed that water had penetrated to the back of the test specimen. With the face side of the test specimen down, the metal hoop was held by one edge and the opposite edge tapped lightly once against the table. Then it was rotated 18 C and similarly tapped again once on the point previously held, to remove any excess water drop. The final step was to compare the wetting of the test specimen with a photographic rating standard and grade accordingly. The same procedure was repeated for five samples and the mean value was calculated for twenty eight samples. 8

48 Plate 25 Tensile Strength Test- Grab Test ASTM Plate 26 Martindale Abrasion Resistance ISO :1999 Plate 27 Random Tumble Pilling Resistance ASTM- 3512/25 Plate 28 rape Coefficient (%) (IS-8357/1977) Plate 29 Stiffness to fabric (IS 649:1971) Plate 3 Water Repellency spray test (AATCC22) 81