Evaluation of different extraction methods for extraction of Eco-colorant

from Pterocarpus marsupium saw dust

K. Nadiya* and Dr.K. Kalaiarasi**

* Ph.D. Research Scholar and **Assistant Professor (SG), Department of Textiles and Clothing,

Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore

Abstract

Pterocarpus marsupium saw dust is experimented to serve as a source of natural dye that could

be utilized in textile dyeing industries. The present study deals with the determination of suitable

extraction technique for natural dye extraction from Pterocarpus marsupium (Vengai in Tamil)

saw dust. The dye was extracted from saw dust using different extraction techniques such as

conventional, enzymatic, magnetic stirring, ultrasonic assisted and enzyme-ultrasonic assisted

extraction methods and the color yield was analyzed using UV-VIS Spectrophotometer. The

selected cotton fabric was dyed with the extracted dye solutions at 900C for 60 minutes in lab

dyer machine. The colour strength of the dyed fabrics was measured using SS 5100H dual beam

spectrophotometer provided by Premier Colorscan Instrument in terms of K/S and CIELAB

colour-difference values. The results proved that Enzyme-ultrasonic assisted extraction method

is the effective method for dye extraction from Pterocarpus marsupium saw dust.

Keywords: natural dyes, Pterocarpus marsupium, saw dust, extraction, magnetic stirring, enzyme, ultrasonic,

enzyme-ultrasonic

1. Introduction

Pterocarpus marsupium, belongs to family Fabaceae commonly known as Malabar kino, Indian

kino tree as a textile colorant, is an evergreen deciduous tree that can grow up to 30 meters tall. It

is native to India such as Andhra Pradesh, Bihar, Gujarat, Kerala, Madhya Pradesh, Maharashtra,

Karnataka, Orissa, Tamilnadu, Uttar Pradesh, and also Nepal, Sri-Lanka. It occurs in parts of the

Western Ghats in the Karnataka-Kerala region and also in the forests of Central India (Das et al.

2011; Mahale et al. 2016). Pterocarpus marsupium is one of the valuable multipurpose forest

trees, in the present study it has been used as a natural colourant, which is primarily used as used

for building furniture, agricultural and railway purpose. Eariler, it was used for dyeing the silk

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cloth and many other colouring works (Gokhale et al. 2004). The aim of this present study is to

investigate the novel processes like enzymatic, magnetic stirring, ultrasonic assisted and enzyme-

ultrasonic assisted extraction methods and extensively study their effectiveness for their edge

over conventional method. The comparative investigation of different extraction technique for

extraction of colorants from Pterocarpus marsupium saw dust has been reported. The extracted

colorant has been used for cotton fabric dyeing. The absorbance of the dye extract and the colour

strength (K/S) of the dyed cotton fabric were also studied.

2. Materials and Methods

2.1 Materials

Pterocarpus marsupium saw dust was collected from the Sivasamy saw mill located at

Alandurai, Coimbatore, India. AR grade chemicals used for extraction such as ethyl alcohol,

acetic acid, sodium carbonate were purchased from Merck and Hi Media Laboratories Pvt. Ltd.

Mumbai. Enzymes pectinase and cellulase were procured from Resil chemicals and stored as per

standard norms.

2.2 Methods

2.2.1 Conventional Extraction Method (CE)

Pterocarpus marsupium saw dust (25g) was soaked overnight in 250ml of 1% alkaline medium

in the addition of sodium carbonate (Selvam et al. 2015) and the mixture was placed in the water

bath heating at constant temperature of 90ºC for 60 minutes and the mixture was filtered using

Whatman No.1 filter paper

2.2.2 Enzyme Assisted Extraction Method (EAE)

A 2% solution of pectinase: cellulase (2:1) was sprayed (Tiwari et al. 2010) on Pterocarpus

marsupium saw dust (25g) for better soaking and contact and left overnight. The enzyme treated

material was washed with little amount of distilled water and soaked overnight in 250ml of 1%

alkaline medium in the addition of sodium carbonate. The mixture was placed in the water bath

heating at constant temperature of 90ºC for 60 minutes and the mixture was filtered using

Whatman No.1 filter paper.

2.2.3 Magnetic stirring Extraction Method (MSE)

Pterocarpus marsupium saw dust (25g) was soaked overnight in 250ml of 1% alkaline medium

in the addition of sodium carbonate and the mixture was placed in the hot plate with magnetic

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stirrer heating at constant temperature of 45ºC for 60 minutes and the mixture was filtered using

Whatman No.1 filter paper.

2.2.4 Ultrasonic Assisted Extraction (UAE)

Pterocarpus marsupium saw dust (25g) soaked overnight in 250ml of 1% alkaline medium in the

addition of sodium carbonate was immersed with ultrasound tip completely hielscher, Ultrasound

technology, UP400S) at constant amplitude of 65% and constant frequency of 100% for 60

minutes . The beaker was covered using aluminum foil to prevent loss of solvent by evaporation

and the mixture was filtered using Whatman No.1 filter paper.

2.2.5 Enzyme-Ultrasonic Assisted Extraction Method (EUAE)

A 2% solution of pectinase : cellulose (2:1) was sprayed on saw dust of Pterocarpus marsupium

(25g) for better soaking and contact and then left overnight.. The enzyme treated material was

washed with little amount of distilled water. This material was then soaked overnight in the

250ml of 1% alkaline medium in the addition of sodium carbonate and the mixture was

immersed with ultrasound tip completely (hielscher, Ultrasound technology, UP400S) at constant

amplitude of 65% and constant frequency of 100% for 60 minutes. The beaker was covered

using aluminum foil to prevent loss of solvent by evaporation (Tiwari et al. 2010) and the

mixture was filtered using Whatman No.1 filter paper.

2.3. UV- VIS Spectrophotometer analysis

The optical density of the filtrate was recorded using Nano Drop, UV-VIS spectrophotometer

(ND-1000) over the range of 200-700nm. The extract was stored at 4 ºC for further use.

2.3. Dyeing experiment

The fabrics were dyed with a material-to-liquor ratio of 1:20. pH of the dye bath was adjusted to

4 using 1 N acetic acid and 1 N sodium hydroxide. The temperature was maintained at 90ºC for

1 hour and dyeing was carried out in lab dyeing machine (SPI Equipments, India). The dyed

fabrics were then rinsed with water, followed by soaping with 2g/l nonionic soap at 60ºC. Finally

the fabric samples were washed thoroughly with cold water and dried.

2.4. Colour measurement and Analysis

The spectral reflectance of the dyed fabric was measured Premier Colorscan. The relative color

strength of the dyed fabric expressed as K/S was measured using the light reflectance technique

using the Kubelka – Munk equation.

K/S = (1-R) ² / 2R

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where K is the absorption coefficient, R is the reflectance of the dyed fabric and S is the

scattering coefficient. The CIELAB Value of the dyed fabric were also measured and recorded

with a tristimulus colorimeter along with standard sample.

3. Results and discussion

3.1. Evaluation of different extraction techniques

These extraction were carried out as per the method described 2.2.1, 2.2.2, 2.2.3, 2.2.4, 2.2.5.

The absorbance values at 360 nm for the dye obtained using the different extraction techniques

are shown in Table – 1

Table 1. Absorbance values analysis

Extraction

techniques

Color yield

(360 nm)

CE 2.758

EAE 2.782

MSE 2.830

UAE 3.078

EUAE 3.288

Natural dye was extracted from Pterocarpus marsupium saw dust by different extraction

techniques. The color yield was assessed by measuring the absorbance at 360 nm. Among the

different extraction techniques, the color yield was found to be maximum in EUAE (3.288)

followed by UAE, MSE, EAE, CE has reported maximum dye yield with Pterocarpus

marsupium saw dust. Hence in the present study EUAE technique was selected for the extraction

of dye.

3.2. Dyed samples

The use of six different extraction techniques with Pterocarpus marsupium extract produced

different shades on cotton fabric which are shown in Figure 1. The dyeing with different

extraction method imparted a shade changes. EUAE method showed a higher depth of shade, as

well as color values, compared with the fabrics dyed using the other five methods.

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Figure 1 Color produced on cotton fabric by different extraction method

Legend : CE - Conventionl Extraction; EAE – Enzyme Assisted Extraction;

MSE – Magnetic Stirring Extraction; UAE – Ultrasonic Assisted

Extraction; EUAE – Enzyme-Ultrasonic Assisted Extraction

Figure. 2 K/S of bark extract dyed from Pterocarpus marsupium on cotton fabrics

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3.3 Color measurements of dyed fabrics

Cotton fabrics dyed with Pterocarpus marsupium saw dust extract were evaluated and the

results of color measurements are shown in Figure-2. The undyed cotton fabric is considered as

the Standard Sample. The K/S value of the conventional extract dyed samples was found to be

3.277, however Enzyme Assisted extraction method improved the dye yield marginally and the

K/S value was found to be 3.296. Out of the other techniques without the addition of enzyme, the

Ultrasound Assisted extraction method yielded the best result in terms of K/S value which is

4.325. Since the enzyme treatment overnight had a significant effect in separation of dye

particles, the Ultrasound method was combined with enzyme treatment to produce the highest

yield overall. Thus Enzyme-Ultrasound Assisted extraction method produced the maximum yield

with an improvement of 274.22 % of color strength and K/S value of 5.673. The Magnetic

stirrer Assisted extraction method was found slightly better than the conventional method with a

K/S value of 3.710. The cotton fabrics dyed using the Pterocarpus marsupium extract obtained

from the different extraction techniques, the order of colour yield was found to be CE < EAE <

MGE < UAE < EUAE. The maximum color strength (K/S) was observed for Enzyme-

Ultrasound Assisted extraction method; It is the best extraction technique for dyeing of cotton

fabric of Pterocarpus marsupium Bark extract.

Quantified colour measurements values of undyed (standard) and dyed cotton fabrics using

CIELAB system are shown Table 2. Fabrics dyed with Pterocarpus marsupium bark extract by

different extraction techniques such as CE; EAE; MGE; MAE; UAE; EUAE were evaluated for

their colour coordinates (L*, a*, b*) values. The results show that the use of different extraction

techniques gave increased depth of colour from the same dye. Figure - 3 shows the colorimetric

values of dyed cotton fabric with Pterocarpus marsupium saw dust extract with six different

extraction methods. The color yield was found to increase gradually from CE to EUAE

extraction method. The EUAE method increased redness quality (a* 1.323) significantly

compared to the other extraction techniques. Again from the b* value was perspective, it was

noticed that the EUAE dyed fabric were more yellower shade (b* 6.963) compared to other

extraction methods. The hue angle lies between 79.210 to 88.046. Hence all the dyed fabrics lie

between the red and yellow shade range with the EUAE method being more reddish shade (H =

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79.210) and CE method being more yellowish (H = 88.046). Higher color difference (dE*) was

noticeable between standard and EUAE dye fabric sample as shown in the Table-2.

Table 2 - CIELAB values for Pterocarpus marsupium bark extract dyed on cotton fabrics

Figure 3- shows the colorimetric values of dyed cotton fabric with

Pterocarpus marsupium saw dust

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4. CONCLUSION

In this work, the effect of extraction methods and possibility of using Pterocarpus marsupium

saw dust in dyeing of cotton fabric using conventional, enzymatic, magnetic, ultrasonic assisted

and enzyme-ultrasonic assisted extraction methods have been studied. The study reveals that

enzyme-ultrasonic assisted extraction method of Pterocarpus marsupium is a more efficient

technique as compared to other extraction method. The maximum K/S value indicates that the

best colorant shade was obtained in enzyme-ultrasonic assisted extraction method. It could be

concluded that the colourant from Pterocarpus marsupium may be a promising eco-friendly dye

for textile dyeing on cotton fabric and enzyme-Assisted Ultrasonic Extration method is best

suited for effective dye extraction reducing the processing time and energy .

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