3. EXPERIMENTAL PROCEDURE - Information and …shodhganga.inflibnet.ac.in/.../4/msumithra_chapter3.pdf3. EXPERIMENTAL PROCEDURE ... done for all the selected twenty herbs and the following

34

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

35

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

36

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)

37

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)

38

Phase 3

MICROENCAPSULATION OF SPECIAL FINISHES AND EVALUATION

Microencapsulation

Best sample D (100% cotton)


Anti Bacterial ENISO 20645

Anti Odor Mosquito Repellency

Pad Dry Cure Method

Evaluation Before, after 10, 20 and 30 washes

Visual Inspection


Scanning electron microscopy [SEM]

Fourier Transform Infrared Spectroscopy [FTIR]

39

Phase 4

NANOENCAPSULATION OF SPECIAL FINISHES AND EVALUATION

Nanoencapsulation

Selected Sample D (100% cotton)

Anti Bacterial ENISO 20645


Pad Dry Cure Method

Evaluation Before, after 10, 20 and 30 washes

Visual Inspection


Scanning electron microscopy [SEM]

Fourier Transform Infrared Spectroscopy [FTIR]

40

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.

41

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

42

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.

43

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

44

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.

45

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.

46

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

49

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


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


Methanol

D

D D D D

D D D D

51

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


Methanol

D D D D

D D D D

52

Plate 11 Antibacterial activity of Tribulus terrestris


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


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


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


Methanol

Plate 18 Antibacterial activity of Kathari flower


Methanol

D D

D D

D D

D D D D

56

Plate 19 Antibacterial activity of Cereus janacaru – Whole plant


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.

58

PLATE 21

Ricinuess communis

Seena Auriculate

Euphorbia Hirta

59

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)


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


60

Plate 22

Results for 10 Combinations for Four selected Denim fabrics


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.

61


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

62

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),



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


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


A2 24 26

B2 24 24

C2 26 25

D2 25 28


A3 25 28

B3 0 28

C3 25 27

D3 0* 27


A4 0* 26

B4 0* 26

C4 24 25

D4 25 28


A5 22 26

B5 0 24

C5 0 26

D5 0 26

63

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



(1:3:2) - (60 grams: 180grams:120 grams)


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.

67

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




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


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%


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%.

75

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.

76

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.

77

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

78

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


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


84

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 .

85

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)


4. FFA20 Multifunctional finished sample after 20 washes (washed sample)


5. FFA30 Multifunctional finished sample after 30 washes (washed sample)


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)






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)






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


100% cotton


100% cotton

21. MD Microencapsulated sample (finished sample) 100% cotton

22. MD10 Microencapsulated sample after 10 washes (washed sample)

100% cotton


100% cotton


100% cotton

25. ND Nanoencapsulated sample (finished sample)

100% cotton

26. ND10 Nanoencapsulated Sample after 10 washes (washed sample)

100% cotton


100% cotton


100% cotton

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Documents

3. EXPERIMENTAL PROCEDURE - Information and …shodhganga.inflibnet.ac.in/.../4/msumithra_chapter3.pdf3. EXPERIMENTAL PROCEDURE ... done for all the selected twenty herbs and the following