3. experimental procedure - information and...
TRANSCRIPT
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3. EXPERIMENTAL PROCEDURE
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 20645
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
3.2.1. Selection of shops and the consumer
3.2.2. Formulation of the interview schedules
3.2.3 Collection of data and consolidation of the data
3.3 Pretreatment
Desizing
3.4 Selection of herbs
3.5 Extraction process of herbs
3.5.1 Drying of herbs
3.5.2 Grinding process
3.5.3 Methanol extraction
3.5.4 Aqueous extraction
3.6 Method of finishing
3.6.1 Preparation of fabric
3.6.2 Finishing of fabric
3.7 Preliminary analysis of qualitative antibacterial activity by ENISO 20645
3.8 Analysis of three selected herbs
3.8.1 Optimization of herbal combinations of the three selected herbs
3.8.2 Standardization of finishing process
PHASE 2 3.9 Optimized parameters
3.10Selection of multifunctional finishes
3.10.1 Application of multifunctional finishes by dip method on four selected fabrics
3.10.2 Analysis of the antibacterial activity on finished samples
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3.10.3 Analysis of the antifungal activity on finished samples
3.10.4 Anti odor evaluation on finished fabric
3.10.5 Application of mosquito repellent finish
PHASE 3 3.11 Application of herbal extracts adopting microencapsulation method.
3.11.1 Microencapsulation of fabric by ionic gelatin process
3.11.2 Finishing of selected fabrics using pad dry cure method
3.11.3 Evaluation of microencapsulated finished fabrics
PHASE: 4 3.12 Application of herbal extract by nanoencapsulation method
3.12.1 Procedure of nanoencapsulation method
312.2 Finishing of selected fabric by pad dry cure method
3.13 Wash durability test
3.14. Evaluation of finished fabric
3.14.1 Visual inspection
3.14.2 Geometrical properties
3.14.2.1 Fabric Count
3.14.2.2 Fabric weight (ISO 3801: 1977)
3.14.2.3 Fabric Thickness (IS 7702: 1975)
3.14.3 Mechanical properties
3.14.3.1 Tensile Strength (ASTM -D -5034: 1995)
3.14.3.2 Abrasion Resistance (ISO 12947 – 2: 1999)
3.14.3.3 Pilling Resistance (ASTM-D 3512/2005)
3.14.4 Comfort properties
3.14.4.1 Drape Coefficient (%) (IS-8357/1977)
3.14.4.2 Air Permeability Test (IS 11056: 1984)
3.14.4.3 Crease Recovery angle (IS 4681: 1981)
3.14.4.4 Stiffness to fabric (IS 6490:1971)
3.14.4.5 Water Repellency spray test (AATCC22)
3.14.5 Absorption properties
3.14.5.1 Water absorbency test (AATCC 79:2007)
3.14.5.2 Sinking test
3.14.5.3 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
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Flow chart of
Phase 1
3.1 Pilot study
Conduct of survey
(B) 68% Cotton &
32% Poly Lycra Poly Lycra
Optimization of Parameters for finishing
Optimized Parameters
(A) 68% Cotton & 32%
Polyester
(C) 68% Cotton & 32% Core Spun Lycra
(D) 100% Cotton
Pretreatment (desizing)
Selected 20 herbs
Selection of fabric
Market survey
Consumer survey
Solvent used for extraction
Proportions for selected 3 herbs
Conditions for finishing
Best 3 herbs
Water and Methanol
10 Combinations followed
5 conditions followed
Ricinus communis (methanol), Senna
Auriculata (methanol) and Euphorbia Hirta
(aqueous)
Ricinus Communis, Senna Auriculata &
Euphorbia Hirta
1:3:2 1 Part of Ricinus
communis, 3 Parts of Senna Auriculata and
2 Parts of Euphorbia Hirta
Standard Conditions (20Kg|cm2
Pressure, 20m| min rpm)
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Phase 2
APPLICATION OF MULTIFUNCTIONAL FINISHES AND EVALUATION
Special finishes (optimized Parameters)
Anti Fungal AATCC 30
Anti Bacterial AATCC 100
Anti Odor Mosquito Repellency
Dip Method
Evaluation for four category properties
Before, after 10, 20 and 30 washes
Visual Inspection
Physical Mechanical Comfort Absorbency
Selected Sample D (100% cotton)
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Phase 3
MICROENCAPSULATION OF SPECIAL FINISHES AND EVALUATION
Microencapsulation
Best sample D (100% cotton)
Anti Fungal AATCC 30
Anti Bacterial ENISO 20645
Anti Odor Mosquito Repellency
Pad Dry Cure Method
Evaluation Before, after 10, 20 and 30 washes
Visual Inspection
Physical Mechanical Comfort Absorbency
Scanning electron microscopy [SEM]
Fourier Transform Infrared Spectroscopy [FTIR]
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Phase 4
NANOENCAPSULATION OF SPECIAL FINISHES AND EVALUATION
Nanoencapsulation
Selected Sample D (100% cotton)
Anti Bacterial ENISO 20645
Anti Fungal AATCC 30
Pad Dry Cure Method
Evaluation Before, after 10, 20 and 30 washes
Visual Inspection
Physical Mechanical Comfort Absorbency
Scanning electron microscopy [SEM]
Fourier Transform Infrared Spectroscopy [FTIR]
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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:
3.2.1. Selection of the shops and the consumer
The market survey was conducted in 50 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.
3.2.2. 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.
3.2.3. Collection of Data and Consolidation of the data
Reddy (2004), 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.
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Selection of material
Based on the survey the following four samples were identified for the further study. Denim
material sample A-68%cotton+32% Polyester, sample B-68%cotton+32% Poly Lycra, sample C-
68%cotton+32% core spun Lycra and sample D -100% 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 D. 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 10
washes, 20 washes and 30 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
Desizing
Desizing 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 (2005).The following recipe was used for desizing the selected A,
B, C and D denim materials.
Recipe
Denim material - 20 meters (each)
M: L ratio - 1meter : 15 liters
Sodium hydroxide - 40 grams
Temperature - 40 -60˚C
PH - 7
Time - 30 minutes
The Desizing was done using the above ingredients, in selected four samples A, B, C, &
D individually for pretreatment. stainless steel vessel was used, In this vessel, 150 liters of soft
water was poured and 40 grams of sodium hydroxide was added and made it dissolved in water
and 20 meters of denim material was immersed and boiled for 30 minutes at boiling temperature
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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 20 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), Datura 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 20 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 (2010) and
joshi et al (2009).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.
3.5.1 Drying 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.
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3.5.2 Grinding process
Dry 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.
3.5.3 Methanol extraction
The following recipe was used for the Methanol extraction of selected 20 herbs
individually.
Recipe
Herbal powder - 6grams
Methanol - 80 ml
Aqueous (distilled Water) - 20 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 (2007), and Sathianarayanan et al (2010).
3.5.4 Aqueous extraction
The following recipe was used for the aqueous extraction of selected 20 herbs.
Recipe
Herbal powder - 6grams
Aqueous (distilled water) - 100 ml
Temperature - Room temperature
Time for incubation - 24 hours
Filter paper - Whatmann no.1 filter paper
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Procedure for aqueous extraction
Six grams of dried herbal powder was mixed in 100ml 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
Dip method for A, B, C and D
Pad-dry-cure method with microencapsulation for 100% cotton and
Pad-dry-cure method with Nanoencapsulation for 100% cotton
The above three methods were followed to finish with the above methanol and aqueous
extraction on the selected fabrics.
3.6.1 Preparation of fabric
The desized 100% cotton and its blended denim material was cut in to 10 cm X 10 cm .This
sample was sterilized with UV rays in a laminar air flow chamber for 30 minutes and this was kept
in a sterile place for further study.
3.6.2 Finishing of fabric
The following recipe was used to finish the four selected fabrics by dip method using the
extracted herbs.
Recipe
Denim Samples - 2.5cm ± 0.1cm diameter
Solvent - The above extracted methanol and aqueous Solvents
Time - 20 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 ± 0.1cm .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.
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3.7 Preliminary Analysis of Qualitative Antibacterial activity ENISO 20645 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
20645 standard.
Test organisms - Escherichia coli ATCC 11229 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 - 0.5 grams
Yeast extract - 0.3 grams
Sodium chloride - 2 grams
Agar –agar - 2.25 grams
Distilled Water - 100 ml
The culture medium was autoclaved at 120 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 30 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.
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The above Antimicrobial finished samples were analyzed by Qualitative and Quantative
method. This method was followed with the reference of Erdem and Yurudu (2008) for this
study.
TABLE 2
Analysis of herbs for antibacterial activity by ENISO 20645
S. No.
Herb used Solvents used for extraction
Antibacterial activity – Zone of Bacteriostasis (mm)
Escherichia coli Staphylococcus aureus
A B C D A B C D
1 Ricinus Communis – Leaves
Aqueous methanol
0 0
0 0
0 0
0 0
0 29
0 25
0 25
0 0
2 Ricinus Communis – Seeds
Aqueous Methanol
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 28
3 Datura metel - Leaves + fruit
Aqueous Methanol
0 0
0 0
0 0
0 0
0 0*
0 0*
0 0*
0 32
4 Aloe Vera – Flower Aqueous Methanol
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0*
5 Abutilon indicum – Leaves
Aqueous Methanol
0 0
0 0
0 0
0 0
0 0
0 0
0 24
0 23
6 Solanum surattense –Leaves
Aqueous methanol
0 0*
0 0
0 0
0 0
0 0*
0 0*
0 0
0 0
7 Coccinia grandis – Fruit Aqueous methanol
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
8 Coccinia grandis – Leaves Aqueous methanol
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
9 Aloe Vera – Leaves Aqueous Methanol
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 28
10 Cardiospermum halicacabum – Leaves
Aqueous Methanol
0 0
0 0
0 0
0 0
0 0
0 0
0 0
27 26
11 Tribulus terrestris – Whole plant
Aqueous Methanol
0 0
0 0
0 0
0 0
0 25
0 0
0 24
0 30
12 Senna auriculata – Leaves Aqueous Methanol
0 0
0 0
0 0
0 0
0 30
0 28
0 28
0 0
13 Cissus quandrangularis – Whole plant
Aqueous Methanol
0 0
0 0
0 0
0 0
0 25
0 25
0 24
0 0
14 Aibizia amara – Leaves Aqueous Methanol
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
15 Leucas aspara - Stem, Leaf and flower
Aqueous Methanol
0 0*
0 0*
0 0*
0 0
0 24
0 24
0 24
0 0
16 Euphorbia hirta - Stem, Leaf and flower
Aqueous Methanol
0 0
0 0
0 0
0 0
0 25
0 26
0 27
0 0
17 Passiflora foetida – Stem, Leaf and flower
Aqueous Methanol
0 0
0 0
0 0
0 0
0 28
0 25
0 27
0 0
18 Kathari flower Aqueous Methanol
0 0*
0 0*
0 0*
0 0
0 0
0 0
0 0
0 0
19 Cereus janacaru – Whole plant
Aqueous Methanol
0 0
0 0
0 0
0 0
0 0
0 0
0 0
25 23
20 Poolapoo-whole plant Aqueous Methanol
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0* - No bacterial growth beneath the test fabric.
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Plate 1 Antibacterial activity of Ricinus Communis – Leaves
Against Escherichia coli against Staphylococcus aureus Water (Aqueous)
Methanol
Plate 2
Antibacterial activity of Water extract Ricinus Communis Seeds, Datura metel and Aloe Vera Flower
Ricinus communis seeds –Water (Aqueous)
Datura metal
Aloe Vera
D D D D
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Plate 3 Antibacterial activity of Methano extract Ricinus Communis Seeds, Datura metel and
Aloe Vera Flower Ricinus Communis seeds - Methanol
Datura metal
Aloe Vera
Plate 4
Antibacterial activity of Water extract Ricinus Communis Seeds, Datura metel and Aloe Vera Flower
Sample D Against Escherichia coli Against Staphylococcus aureus
Water (Aqueous)
Methanol
D
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Plate 5 Antibacterial activity of Abutilon indicum - Leaves
Against Escherichia coli Against Staphylococcus aureus Water (Aqueous)
Methanol
Plate 6 Antibacterial activity of Solanum surattense –Leaves
Against Escherichia coli Against Staphylococcus aureus Water (Aqueous)
Methanol
D D D D
D D D
D
50
Plate 7 Antibacterial activity of Coccinia grandis - Fruit
Against Escherichia coli Against Staphylococcus aureus
Water (Aqueous)
Methanol
Plate 8 Antibacterial activity of Coccinia grandis – Leaves
Against Escherichia coli Against Staphylococcus aureus Water (Aqueous)
Methanol
D
D D D D
D D D D
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Plate 9 Antibacterial activity of Aloe vera – Leaves
Against Escherichia coli Against Staphylococcus aureus Water (Aqeous)
Methanol
Plate 10 Antibacterial activity of Cardiospermum halicacabum – Leaves
Against Escherichia coli Against Staphylococcus aureus Water (Aqueous)
Methanol
D D D D
D D D D
52
Plate 11 Antibacterial activity of Tribulus terrestris
Against Escherichia coli Against Staphylococcus aureus Water (Aqueous)
Methanol
Plate 12
Antibacterial activity of Senna aurriculata -Leaves Against Escherichia coli Against Staphylococcus aureus
Water (Aqueous)
Methanol
D D D D
D D D
D
53
Plate 13 Antibacterial activity of Cissus quandrangularis – Whole plant
Against Escherichia coli Against Staphylococcus aureus Water (Aqueous)
Methanol
Plate 14 Antibacterial activity of Aibizia amara – Leaves
Against Escherichia Coli Against Staphylococcus aureus Water (Aqueous)
Methanol
D D D D
D D D D
54
Plate 15 Antibacterial activity of Leucas aspara - Stem, Leaf and flower
Against Escherichia coli Against Staphylococcus aureus Water (Aqueous)
Methanol
Plate 16
Antibacterial activity of Euphorbia hirta - Stem, Leaf and flower Against Escherichia coli Against Staphylococcus aureus
Water (Aqueous)
Methanol
D
D D D
D
D D D D
55
Plate 17 Antibacterial activity of Passiflora foetida – Stem, Leaf and flower
Against Escherichia coli Against Staphylococcus aureus Water (Aqueous)
Methanol
Plate 18 Antibacterial activity of Kathari flower
Against Escherichia coli Against Staphylococcus aureus Water (Aqueous)
Methanol
D D
D D
D D
D D D D
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Plate 19 Antibacterial activity of Cereus janacaru – Whole plant
Against Escherichia coli Against Staphylococcus aureus Water (Aqueous)
Methanol
Plate 20
Antibacterial activity of Poolapoo Against Escherichia coli Against Staphylococcus aureus
Water (Aqueous)
Methanol
D D D D
D D D D
57
Table 2 and Plates 1-20 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
S. No Scientific Name Parts used
Common Name
(English)
Common Name
(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 20645 test method after it was conducted with 20 medicinal herbs and
photographs of the plants as shown in plate 21.
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3.8.1 Optimization of herbal combinations of the selected three herbs:
Methanolic extract of Ricinus communis, Methanolic 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 20645. Antimicrobial activity against Gram-positive bacteria (Staphylococcus aureus)
and Gram-negative bacteria (Escherichia coli) was tested according to ENISO 20645 test
method.
The following Table 4 shows that Analysis of Antibacterial activity on selected herbal
combinations by ENISO 20645
Table 4
Proportion of three herbs by Ricinus Communies: Senna auriculata: Euphorbia hirta and
the activity of antibacterial
Sl. No Combinations
Zone of Inhibition (mm)
Escherichia coli Staphylococcus aureus
Ratio of herbs A B C D A B C D
1. 1:1:1 0 0 0 0 23 23 23 0
2. 1:2:1 0 0 0 0 23 23 24 23
3. 2:1:1 0 0 0 0 0 0* 0* 0*
4. 1:1:2 0 0 0 0 0 0 0 24
5. 2:2:1 0 0 0 0 0* 23 0 0
6. 1:2:2 0 0 0 0 0* 23 23 23
7. 2:1:2 0 0 0 0 23 24 23 23
8. 3:1:2 0 0 0 0 23 0 0 0
9. 1:3:2 0 0 0 0 23 25 25 25
10. 1:2:3 0 0 0 0 0 0 0 23
0* - No bacterial growth beneath the test fabric.
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Plate 22
Results for 10 Combinations for Four selected Denim fabrics
Escherichia coli Staphylococcus aureus
1A, 1B, 1C, and 1D- 1 part of ricinus communies, 1 part of senna auriculata and 1 part of euphorbia hirta, 2A, 2B, 2C and 2D- 1 part of ricinus communies, 2 part of senna auriculata and 1 part of euphorbia hirta, 3A, 3B, 3Cand3D- 2 part of ricinus communies, 1 part of senna auriculata and 1 part of euphorbia hirta. 4A, 4B, 4Cand4D- 1 part of Ricinus Communies, 1 part of Senna auriculata and 2 part of Euphorbia hirta. 5A, 5B, 5Cand5D- 2part of Ricinus Communies, 2 part of Senna auriculata and 1 part of Euphorbia hirta. 6A, 6B, 6Cand 6D- 1 part of Ricinus Communies, 2 part of Senna auriculata and 2 part of Euphorbia hirta.
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Escherichia coli Staphylococcus aureus
7A, 7B, 7Cand7D- 2 part of Ricinus Communies, 1 part of Senna auriculata and 2 part of
Euphorbia hirta. 8A, 8A, 8B, 8C and8D- 3 part of Ricinus Communies, 1 part of Senna auriculata
and 2 part of Euphorbia hirta. 9A, 9B, 9Cand9D- 1 part of Ricinus Communies, 3 part of Senna
auriculata and 2 part of Euphorbia hirta. 10A, 10B, 10Cand10D- 1 part of Ricinus Communies, 2
part of Senna auriculata and 3 part of Euphorbia hirta
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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. 20-kgf/cm2 pressure (20 m/min rpm),
2. 20-kgf/cm2 pressure (30 m/min rpm),
3. 30-kgf/cm2 pressure (20 m/min rpm),
4. 30-kgf/cm2 pressure (30 m/min rpm) and
5. 40-kgf/cm2 pressure (20 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
20645
Table –5
Analysis of antibacterial activity by ENISO 20645
0* - No bacterial growth beneath the test fabric.
Plate 23
Conditions for Finishing Pressure (Kgf/cm
2) and rpm
Samples
Zone of Bacteriostasis (mm)
Escherichia coli Staphylococcus
aureus
20kgf/cm2, 20m/min (1)
A1 25 28
B1 24 28
C1 24 31
D1 25 27
20kgf/cm2, 30m/min (2)
A2 24 26
B2 24 24
C2 26 25
D2 25 28
30kgf/cm2, 20m/min (3)
A3 25 28
B3 0 28
C3 25 27
D3 0* 27
30kgf/cm2, 30m/min (4)
A4 0* 26
B4 0* 26
C4 24 25
D4 25 28
40kgf/cm2, 20m/min (5)
A5 22 26
B5 0 24
C5 0 26
D5 0 26
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Analysis of Antibacterial activity by ENISO 20645 for the fabrics finished under five
different conditions
Against Escherichia coli Against Staphylococcus aureus
A1-20kgf/cm2, 20m/min, A2-20kgf/cm
2, 30m/min, A3-30kgf/cm
2, 20m/min, A4-30kgf/cm
2,
30m/min, A5-40kgf/cm2, 20m/min and B1 20kgf/cm
2, 20m/min
B2-20kgf/cm2, 30m/min, B3-30kgf/cm
2, 20m/min, B4-30kgf/cm
2, 30m/min and B5-40kgf/cm
2,
20m/min, C1-20kgf/cm2, 20m/min, and C2-20kgf/cm
2, 30m/min
64
C3-30kgf/cm2, 20m/min, C4-30kgf/cm
2, 30m/min and C5-40kgf/cm
2, 20m/min
D1-20kgf/cm2, 20m/min, D2-20kgf/cm
2, 30m/min, D3-30kgf/cm
2, 20m/min, D4-30kgf/cm
2,
30m/min and D5-40kgf/cm2, 20m/min
65
PHASE: 2
3.9 Optimized parameters.
After conduct of Pilot study, the following parameters were selected for three herbs such
as Methanolic extract of Ricinus communis, Methanolic 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 20Kg|cm2
Pressure,
20m| min rpm was selected.
3.10 Selection of multifunctional finishes
The phase 2 consisted of application of multi functional finishes such as anti bacterial
finish using ENISO 20645 standard method and anti fungal finish was applied by AATCC 30
standard method ,anti odor, mosquito repellency finish was given by dip method. The evaluation
was done after 10, 20, 30 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 20645 tests for the accurate value.
3.10.1Application of multifunctional finishes on selected four fabrics
The dip method was followed to impart multifunctional finishes on selected A, B, C and D
fabrics.
Recipe
Desized Denim Fabric - 6 meters (each)
Herbal powder - 360 grams
(1:3:2) - (60:180:120)
Material liquor ratio - 6meters:6 liters
Test organisms - Escherichia coli ATCC 11229
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 30 minutes
The four selected materials namely A, B, C and D were treated with the herbal extract .
The fabric sample of 2.5cm ± 0.1cm diameter was taken for the analysis. Both sides of the
sample were surface sterilized with UV rays for 30 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 11229 and staphylococcus aureus ATCC 6538 was swabbed over the
66
surface of nutrient agar plate. Sterile samples A, B, C and D 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.
3.10.2 Analysis of the Antibacterial activity on finished sample
The following method AATCC 100 was followed to evaluate the antibacterial activity on the
finished 4 fabrics .This method was more accurate to evaluate antibacterial activity.
Recipe
Desized Denim Fabric - 6 meters (each)
Herbal powder - 360 grams
(1:3:2) - (60 grams: 180grams:120 grams)
Material liquor ratio - 6meters:6 liters
Test Organism Used - Escherichia coli ATCC 11229
Staphylococcus aureus ATCC 6538
Initial inoculums - E. coli – 2.7 X 109 cfu/ml
S. aureus – 2.6 X 109 cfu/ml
Culture medium used - Bacteriostasis sterile agar broth
Test specimens - 5.0 cm diameter
Temperature - 37 ºC
Time - 24 hours
Sterilization - UV rays by laminar air flow Chamber for 30 minutes
Procedure
About five cm diameter of the finished fabric was taken.100 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 0.1 ml inoculums of Escherichia coli
ATCC11229 (gram negative) was added, in the third flask 0.1 ml of Staphylococcus
aureusATCC6539 (gram positive) inoculums was added, in the fourth flask five cm diameter of
the finished fabric was put in 0.1 ml of Escherichia coli ATCC11229 inoculums, In the fifth flask
five cm diameter of finished fabric was added along with 0.1 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.
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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 1:20 lakh microorganism with 0.1 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 100/ 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.
3.10.3 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 30 for the accurate value.
Recipe
Desized Denim Fabric - 6 meters (each)
Herbal powder - 360 grams
Material liquor ratio - 6meters:6 liters
Test organisms - Aspergillus Niger
Culture medium used - inoculums of 1.0ml
Test specimens - 2cm ± 0.1cm diameter
Temperature - 28ºC
Time - for seven days
Sterilization - UV rays by Laminar flow chamber for 15 Minutes.
Procedure
Inoculums of 1.0ml were evenly distributed over the surface of the nutrient agar. The
fabric sample was pre wetted (not rubbed or squeezed) in water containing 0.05% of a non-ionic
wetting agent (triton X- 100) and placed on the agar surface. The inoculums of 0.2 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 (40X) and
interpreted as follows:
No growth (If present, the size of the growth free zone in mm was reported)
68
Microscopic growth (visible only under the microscope)
Macroscopic growth (visible to the naked eye).
3.10.4 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 0 to
10(10-Ideal, 9-Excellent, 8-Very Good, 7-Good, 6-Fairly Good, 5-Acceptable, 4-Fair, 3-Poorly
Fair, 2-Poor, 1- Very Poor and 0 – Repulsive) and was given to the judges for evaluating the
effect of odor finish in the socks.
3.10.5 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.
Description 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 latex-
sealed 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 30 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.
69
Plate 24
Excito chamber used for test the Mosquito repellency efficiency
Efficiency of Mosquito repellency (%) = 100 exposedMosquitoofNo.
deadMosquitoofNo. escapedMosquitoofNo.
PHASE 3
From the dip method it was concluded that 100% 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 100% cotton denim was used
for finishing.
3.11 Application of herbal extracts adopting micro encapsulation method.
In phase 3 the herbal extraction was microencapsulated and applied on 100% cotton
denim fabric(D) by pad dry cure method to get antibacterial, antifungal, anti odor and mosquito
repellency finishes and this was evaluated after 10,20 and 30 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.
3.11.1 Micro encapsulation of fabric by ionic gelatin process
Preparation of Microencapsules
Micro encapsulation method was followed as said by Sathianarayanan et al (2010).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
70
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 (2010).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 (2008). The microencapsules were applied on the
fabric by pad dry cure method.
Recipe
Denim Fabric - 4 meters
Herbal powder (core) - 240 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 100 ml of
hot water. To this mixture 50 ml of hot water was added and stirred for 15 minutes maintaining
the temperature between 40°C and 50 °C. to this mixture, 10 ml of core material sodium alginate
was added and this was transferred to a centrifuge and rated at 300-500 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.
3.11.2 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 non-
toxicity. 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
71
Mulasavalagi (2005). Citric acid was used as a binder to fix the finishing permanently on the
fabric.
Recipe
Denim fabric - 4 Meter (100% Cotton)
Microcapsules - 2%
Binder (Citric acid) - 8%
Temperature - 55˚C
Time - 30 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.
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.
BATH
LOSS
FABRIC
ROLLER MANGLAR
FABRIC
72
3.11.3 Evaluation of microencapsulated finished fabrics
The selected multi-functional finishes such as ,anti bacterial finish using ENISO 20645
standard method ,anti fungal finish by AATCC 30 standard method, anti odor, mosquito
repellency finish was done by micro encapsulation technique on selected 100% 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 10, 20 and 30 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: 4
3.12 Application of herbal extract with Nanoencapsulation method
In phase 4 the herbal extraction was nano encapsulated and applied on 100% cotton
denim fabric (D) by pad dry cure method to get antibacterial and antifungal finish, and this was
evaluated after 10, 20 and 30 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.
3.12.1 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
Denim fabric - 4 meter (100% cotton)
Herbal powder (core material) - 96 grams
Material: Liquor ratio - 1:20
Bovine serum albumin (wall) - 2% W/V
Binder (Citric acid) - 8%
Temperature - 55 ˚C
Time - 30 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 (10,000 rpm) and then suspended
in 0.1M phosphate buffer and the pH was maintained at 7.4, then lyophilized with mannitol
(2% w/V).
73
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 10,000 rpm and the
temperature was maintained at 4ºC. Pellets of nanocapsules thus obtained, were then suspended
in phosphate buffer (pH -7.4; 0.1 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 20645 test method.
3.12.2Finishing of selected fabric by pad dry cure method
Recipe
Denim fabric - 4 Meter (100% Cotton)
Nanocapsules - 2%
Binder (Citric acid) - 8%
Temperature - 55˚C
Time - 30 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.
74
3.13 Wash durability test
The greatest influence was made by washing. During 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 (2006). 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
20645 test methods.
3.14. Evaluation of finished fabric
3.14.1 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 50 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.
3.14.2 Geometrical properties
3.14.2.1 Fabric Count
Fabric count was measured using counting glass according to ASTM D 3775-03
standard, point out Das and Kothari (2012). 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 (2010).
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.
3.14.2.2 Fabric weight (ISO 3801: 1977)
Fabric weight was measured according to ASTM Test Method D3776-96 say Sarkar
(2004). 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/TR5090, 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 0.1%.
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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.
3.14.2.3 Fabric Thickness (IS 7702: 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 (2009).
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 30 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.
3.14.3 Mechanical properties
3.14.3.1 Tensile Strength (Kg) (ASTM -D -5034: 1995)
Akshay et al (2011) states that the Tensile strength was measured according to ASTMD
1682 Procedure. Fabric Tensile Strength (Kg) (ASTM -D -5034: 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.
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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 0.5% 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.
3.14.3.2 Abrasion Resistance (ISO 12947 – 2: 1999)
Abrasion tests were performed on a Martindale Abrasion Tester as referred by Ulku et al
(2003).Abrasion was just one aspect of wear and was the rubbing away of the component fibers
and yarns of the fabric, notes Basu (2006).The Abrasion Resistance (ISO 12947 – 2: 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 50000, the test was
interrupted every 50000rubs, or earlier if required, in order to renew the abrading. In case where
the interruption occurred before the completion of 50000 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.
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3.14.3.3 Pilling Resistance ASTM-D 3512/2005
According to Gokarneshan et al (2011), the pilling resistance of the samples was measured
using ICI Pill box tester using IS: 10971-1984 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-D 3512/2005 (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 (0.2-in.) denim
fabric into the test chamber. The chamber was covered, and the timer set for a running time of 30
min. the motor was switched “ON,” the “START” button pushed, and the air flow started. During
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.
3.14.4 Comfort properties
3.14.4.1 Drape Coefficient (%) (IS-8357/1977)
According to BS-5058/1973, 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
(2007). Fabric drape was the hanging property of the fabric and is inversely proportional to drape
coefficient of the fabric, say Tyagi et al (2011).
The Drape Coefficient [(%) (IS-8357/1977) (Plate -28)] was used to measure the drape
of the fabric. Drape 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
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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.
Drape co-efficient (F %) = W/w-a / A-a *100
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
Drape 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.
3.14.4.2 Air Permeability Test (IS 11056: 1984)
The air permeability was defined as the volume of air in milliliters which was passed in one
second through 100 smm2 of the fabric at a pressure difference of 10 mm head of water by
Tugrul Ogulata (2006). Air Permeability Test (IS 11056: 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.
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3.14.4.3 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 (2005). 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 (2009). 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 0.5 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.
3.14.4.4 Stiffness to fabric (IS 6490:1971)
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
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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:
1964-197I 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 (2011), the pierce cantilever test was
performed on the Shirley stiffness tester. Flexural rigidity of the fabric samples was calculated as
per the ASTMD 1388-96 using Shirley fabric stiffness tester, say Saravanan et al (2011).
3.14.4.5 Water Repellency spray test (AATCC22)
According to Ghosh (2011), the standard test method for the water repellency
measurement of woven textile fabrics was used (SIST EN4920).
Water Repellency spray test (AATCC22) (plate -30) 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, 250 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 - 30 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 180°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.
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Plate 25 Tensile Strength Test- Grab
Test ASTM D 5034-95
Plate 26 Martindale Abrasion
Resistance ISO-12947-2:1999
Plate 27 Random Tumble Pilling
Resistance ASTM-D 3512/2005
Plate 28 Drape Coefficient (%)
(IS-8357/1977)
Plate 29 Stiffness to fabric (IS 6490:1971)
Plate 30 Water Repellency spray test
(AATCC22)
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3.14.5 Absorption tests
3.14.5.1 Water absorbency test (AATCC 79:2007)
Drop absorbency of the samples was calculated as per the AATCC test method 79-2000,
as denoted by Saravanan et al (2011). The test method for the determination of the water
absorbency of fabric was performed in the standard atmosphere for testing burette, 10±0.05 mL
with 0.5 mL graduations that allow a delivery rate of 15-25 drops per milliliter. A location in the
conditioned laboratory area that had overhead lighting to facilitate the judgment of the test end
point was selected; i.e. wetting. The burette’s stop clock position that will deliver the specified
number of water drops was determined.
A specimen was mounted in an embroidery hoop, so that the side of the specimen to be
tested was up, and the surface specimen was taut and free of wrinkles but without stretching or
distorting the structure of the fabric. The embroidery hoop with the specimen surface 10+-1.0mm
(0.375+-0.04 in) was placed below the tip of the burette and one drop of distilled or deionized
water was allowed to fall on the cloth. The stopwatch (or) timer was started immediately. The
water drop was observed without moving the beaker with the specimen from under the burette to
avoid disturbance of the water drop and its interface with the specimen surface.
The timer (or) stopwatch was stopped, when the drop of water lost its reflectivity. If the
water drop did not immediately disappear, the water drop was observed from other positions until
it finally vanished. The end point would be the time, less than 60s it took for the water drop, which
no longer reflected light and appeared only as a dull wet spot.
The elapsed time to the nearest second was recorded. If the water drop vanished
immediately, it was recorded as “zero”. If the wetting time exceeded 60s,the time was recorded
as “60+s”.the same steps were repeated for the additional four test locations. The same
procedure was repeated for five samples and the mean value was calculated for twenty eight
samples.
3.14.5.2 Sinking test (In house method)
One very important dimensional change in apparel which occurs when a fabric was
washed known as shrinkage, pointed out Mittu and Dedhia (2012).Sinking involved a simple test
for wet ability of fabric. At least 4 samples of the size 1x1 were cut. Each sample was kept on the
surface of water in a 500ml glass beaker. Time taken by the piece to sink just beneath the water
surface was measured. A sinking time of about 5sec was generally considered satisfactory for
well prepared Cellulose materials. The time required by the hank to go inside the water from
floating state is known as sinking time. Low sinking time indicates rapid wetting because of good
sourcing. The same procedure was repeated for five samples and the mean value was calculated
for twenty eight samples.
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3.14.5.3 Wickability test
In this method, wick up was observed by determining the rate of time at which the water
moved upward on a fabric strip as per BS3424, say Kandhavadivu and Ramachandran (2011).
The rate (distance per unit of time) at which liquid travels along, or through a fabric specimen is
visually observed, manually timed and recorded at specific intervals.
Measuring time at a given distance
Using a marking pen with soluble ink, a line across the end of each specimen at a
distance of 5±1mm from the end of the fabric side to be tested, was marked. The 5 mm line
denoted the level to which a specimen was to be lowered in the water in the flask (or) beaker
which was the test start time.
Using a marking pen with soluble ink, and measured from the 5±1mm line, lines were
marked across the width of the specimen at distances of 20±1 and 150±1mm. To facilitate the
measurement of wicking distances, intervals of 10± mm were marked along the specimen length
between the 20± 1 mm and 150± 1mm lines.
Alternative wicking distances may be used depending on the desired end use of the fabric.
When comparing results, the same wicking distance bench mark should be used.
To determine the amount of water for the test, the extra specimens was used, and
positioned at the opening of an Erlenmeyer flask by the insertion of a straight pin (or) other device
near the end of the specimen. The specimen was allowed to hang in to the flask. Water was
added up to the level at which the specimen’s 5± 1mm line was reached; and then the required
water level marked on the outside of the flask to remain dry, to prevent premature bleeding of
soluble ink marks on the specimen.
The flask was filled with distilled (or) deionized water to the line marked as instructed.
The specimen was inserted into the flask, the scissor jaw raised to position the specimen so that
the water was at the 5± 1 mm line. Alternatively the approximate amount of water required may
be added to a flask, for determining and marking a water level fill line on the outside of a flask, a
pipette may be used to raise the water level to the appropriate height. A clean flask with fresh
water was used for testing subsequent samples.
The stop watch (or) timer was started as soon as the water reached the 5±mm line and
the soluble ink began to migrate upwards. the rise of the water was monitored, time it took for the
soluble ink at the marked 20±1mm line to migrate was recorded to the nearest second. the same
test was administered for the remaining specimens. The same procedure was repeated for five
samples and the mean value was calculated for twenty eight samples.
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3.15 SEM analysis for the best sample
The scanning electron microscope was an electron microscope that images the sample
surface by scanning it with a high energy beam of electrons pointed by Bhattacharyaa et al
(2008). The surface of the fabric was photographed. The extracted molecules of herb had fixed in
to the yarns of the fabric to a maximum amount, as pointed by Krishnaveni and Amsa Mani
(2012). The scanning electron microscopy was used for confirming the binding of
microencapsules and alignment on to the fabric sample.
Scanning Electron Microscope is used to identify morphological structure of specimens
(fiber, yarn or fabric) under investigation. SEM evaluation is also used to know the uniformity of
coating of finishing over the specimen, The SEM photographs of microencapsulated,
nanoencapsulated and washed samples were examined under different magnifications
3.16 FTIR analysis for the best sample
Fourier transform infrared spectroscopy (FTIR) was an analytical tool to identify the
nature of chemicals that are coated on the fabric specimen. It also helps to know to what extent
the molecules of the finishing chemicals are attached with fiber molecules of the specimen. The
samples were analyzed for their variations in chemical groups using FTIR spectroscopy. The
same test was carried out by Usha et al (2010).Infrared spectroscopy was used to identify and
quantitatively analyze chemical compounds, mixtures, extent of reaction, and molecular structure.
Different chemical compounds absorb infrared radiation at frequencies corresponding to their own
molecular vibration frequencies, as referred by Yadav and Sangeeta (2009).According to Kale
and Desai (2011), Infrared (IR) spectroscopy is a chemical analytical technique which measures
the absorption of different IR frequencies by a sample positioned in the path of an IR beam. The
main goal of IR spectroscopic analysis was to determine the chemical functional groups in the
sample. Different functional groups absorb characteristic frequencies of IR radiation.
To ascertain the activity of herbs in micro encapsulation and nano encapsulation technique
and after 10, 20 & 30 washes of the fabrics, FTIR spectrum were recorded on shim at 2u.FTIR-
8000/400 S modal spectrometer in the regain 4000-400 cm-1 using kbr discussing FTIR spectra
the samples were analyzed for their variation in chemical groups.
3.17 Statistical analysis of the study
The findings of unwashed and washed (10, 20 and 30) samples were analyzed using one
way ANOVA for the multifunctional finishes. The Micro encapsulation and Nanoencapsulation
samples were analyzed statistically with T test .The ANOVA and T test were used to determine
whether there were any differences between groups and with in groups of the samples. Mahesh
et al(2011),also used one way ANOVA test .
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13.18 Nomenclature Table 6
S.No Fabric samples Fabric samples Abbreviations
1. A original sample 68%cotton+32% polyester
2. FFA1 Multifunctional finished sample (unwashed finished sample)
68%cotton+32% polyester
3 . FFA10 Multifunctional finished sample after 10 washes (washed sample)
68%cotton+32% polyester
4. FFA20 Multifunctional finished sample after 20 washes (washed sample)
68%cotton+32% polyester
5. FFA30 Multifunctional finished sample after 30 washes (washed sample)
68%cotton+32% polyester
6. B original sample 68%cotton+32% Poly Lycra
7. FFB1 Multifunctional finished sample (unwashed finished sample)
68%cotton+32% Poly Lycra
8. FFB10 Multifunctional finished sample after 10 washes (washed sample)
68%cotton+32% Poly Lycra
9. FFB20 Multifunctional finished sample after 20 washes (washed sample)
68%cotton+32% Poly Lycra
10. FFB30 Multifunctional finished sample after 30 washes (washed sample)
68%cotton+32% Poly Lycra
11. C original sample 68% cotton+32% core Spun lycra
12. FFC1 Multifunctional finished sample (unwashed finished sample)
68% cotton+32% core Spun lycra
13. FFC10 Multifunctional finished sample after 10 washes (washed sample)
68% cotton+32% core Spun lycra
14. FFC20 Multifunctional finished sample after 20 washes (washed sample)
68% cotton+32% core Spun lycra
15. FFC30 Multifunctional finished sample after 30 washes (washed sample)
68% cotton+32% core Spun lycra
16. D original sample 100% cotton
17. FFD1 Multifunctional finished sample (unwashed finished sample)
100% cotton
18. FFD10 Multifunctional finished sample after 10 washes (washed sample)
100% cotton
19. FFD20 Multifunctional finished sample after 20 washes (washed sample)
100% cotton
20. FFD30 Multifunctional finished sample after 30 washes (washed sample)
100% cotton
21. MD Microencapsulated sample (finished sample) 100% cotton
22. MD10 Microencapsulated sample after 10 washes (washed sample)
100% cotton
23. MD20 Microencapsulated sample after 20 washes (washed sample)
100% cotton
24. MD30 Microencapsulated sample after 30 washes (washed sample)
100% cotton
25. ND Nanoencapsulated sample (finished sample)
100% cotton
26. ND10 Nanoencapsulated Sample after 10 washes (washed sample)
100% cotton
27. ND20 Nanoencapsulated Sample after 20 washes (washed sample)
100% cotton
28. ND30 Nanoencapsulated Sample after 30 washes (washed sample)
100% cotton