International Journal of Modern Chemistry, 2015, 7(2): 81-90

International Journal of Modern Chemistry ISSN: 2165-0128

Journal homepage: www.ModernScientificPress.com/Journals/IJMChem.aspx Florida, USA
Article

Extraction of Dyestuff from Justicia carnea hooker and Its

Application in the Dyeing of Wool, Leather and Cotton

Feka D.P. 1,*, Abraham A.D., 2B. Myek, 1Dada J.S., 1Israel Joshua 3Nkwatoh Ferdinand
1
Nigerian Institute of Leather and Science Technology (NILEST), Samaru-Zaria, Nigeria
2
Department of Chemistry, Kaduna State University, Nigeria
3
Mile 2, Nkwen-Bamenda, Cameroun

* Author to whom correspondence should be addressed; E-Mail: [email protected]

Article history: Received 2 January 2015, Received in revised form 28 March 2015, Accepted 15 June
2015, Published 22 June 2015.

Abstract: Dye was extracted from whole plant of Justicia carnea hooker, using soxhlet
extraction method. The dyestuff extracted gave a percentage yield of 92.8% and was
successfully applied on leather, cotton, and wool. The extracted dye showed solubility in
distilled water, HCl, H2SO4, ethanol and NaHCO3 respectively. Dye extract also shows a
pH 9, TLC revealed blue, green and yellow colours with RF values of 0.83, 0.86 and 0.89,
λmax was 480 and gave a green shade. Sulphanilic diazonium chloride was used as the
coupler and it produced a brown shade in each of the substrates applied on and fastness test
gave good result. pH for the coupled dye was 8.2 while TLC revealed yellow and orange
colours with RF values of 0.98 and 0.95 respectively. λmax obtained were 400nm and
480nm. Acid fastness, alkaline fastness, sunlight fastness and wash fastness of coupled dye
were determined and compared to a standard Gray Scale rating. Thin layer chromatography
carried out showed that dyestuff can be extracted from Justicia carnea hooker.

Keywords: Dye, Fastness, Extraction, Solubility.

1. Introduction

About 1,100 plant species can be used for dyeing [1]. Therefore it is an important aim in
research to screen and select species which fit for modern sustainable cultivation techniques as well as

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Int. J. Modern Chem. 2015, 7(1): 81-90 82

for dyeing on a large scale. At the Thüringer Landesanstalt für Landwirtschaft (Germany), 108 dye
plant species are assessed on the basis of their suitability for modern cultivation systems, on yields,
and on dyeing quality. Of these species, 19 species were considered as useful for cultivation and
dyestuff production. Madder (Rubia tinctorum), Weld (Reseda luteola), Canadian Golden Rod
(Solidago canadensis), Dyer’s Chamomile (Anthemis tinctoria), and Dyer’s Knotweed (Polygonum
tinctorium) are considered to play a decisive role in future dye plant cultivation and processing [2].
Nevertheless, other species may also become important for dyeing, as the recent example of Rhubarb
(Rheum rhabarbarum) shows: it is perfectly suitable for the dyeing and tanning of leather and is
already used in practice by one company [3].
A dye is a colored substance that has an affinity for the substrate to which it is being applied. It
is generally applied in an aqueous solution, and requires a mordant to improve the fastness of dye on
the fibre [4]. Both dyes and pigments appear to be colored because they absorb some wavelengths of
light more than others .In contrast with a dye, a pigment generally is insoluble, and has no affinity for
the substrate. Some dyes can be precipitated with an inert salt to produce a lake pigment, and based on
the salt used; they could be Aluminum Lake, Calcium Lake, or barium lake pigments [5]. Research has
shown that the natural dyes are quite safe and environment friendly [6].
The use of plants for dyeing is environmental friendly. Synthetic dyes have been widely used all
around the world, and the demand for natural dye product is on the increase. Hence natural dye will
succeed once more. The aim of this work is to extract the dye and apply it on cotton, leather and wool

2. Methodology

2.1. Sample Collection

The stem of plant justicia carnea hooker was brought in from Bamenda (Cameroun) in 2013
and planted at Graceland, Zaria, Kaduna state, in Nigeria, from where the plant was collected and
prepared for the analysis.

2.2. Sample Preparation

The sample was collected and dried at room temperature (room drying) after which it was
grinded into fine particles using mortar and pistil, and then sieved using 0.01 mm sieve.

2.3. Extraction of the Dye of Justicia carnea hooker Using Soxhlet Method

The extraction of dye from justicia carnea hooker was carried out using soxhlet extraction
method. The sample was weighed (50g) and transferred into a timbling chamber of the apparatus,
using methanol and water as solvents. The extraction was carried out based on solid-liquid extraction,

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Int. J. Modern Chem. 2015, 7(1): 81-90 83

a type of continuous extraction. The sample was placed in the porous thimble and inserted into the
inner tube. The extractor was then fitted to the bolt head flask containing the solvent and the reflux
condenser. The solvent boiled gently as the vapour passed through the tube while it condenses and the
condensed solvent falls into the thimble and slowly filled the body of the soxhlet. When the solvent
reaches the siphoning point, it siphoned over the flask and thus removes that portion of substances
which it has extracted. The process repeated automatically until complete extraction was achieved. The
extracted compound was then isolated from it solution by using a calibrated evaporating dish.

2.4. Preparation of Diazonium Salt

2.5g of sulphanilic acid powder was weighed and dissolved in 50ml of distilled water then
0.75g sodium carbonate was weighed and added gradually into the solution and stirred while heating at
a very low temperature for 10 minutes then it was labeled sample A then 1.8g sodium nitrite (NaNO 2)
was dissolved in 10ml distilled water and was labeled sample B. Then sample A was placed in an ice
water bath and sample B was added gradually to the cold solution of sample A and was stirred
constantly in a fume cupboard until sample B was completely added into sample A and the mixture
was allowed to stand for 30 minutes in an ice water bath then 10ml of concentrated hydrochloric acid
was measured and diluted into 10ml distilled water and the solution was gradually added to sample A,
and a starch iodide paper was used to confirm the end point of the reaction.

2.5. Coupling Reaction of the Dye

1g of the dye extract was weighed and dissolved in 10ml distilled water in a beaker then 20%
sodium hydroxide(20ml) was measured and added to the solution and cooled in ice water bath for 30
minutes. The sulphanilic diazonium chloride was gradually added to the solution of the extract and
stirred continuously in a fume cupboard until it was completely added and the mixture was filtered into
a flat bottom flask using a filter paper and the filtrate was poured into an evaporating dish and
concentrated by placing in an oven for 24hours at 60oc.

2.6. Characterization

The dye extract was analyzed for its solubility, functional group present and the absorbance.

2.7. Solubility Test

The coupled dye was dissolved in different media respectively, to test for its solubility. The
coupled dye (0.2g) was weighed and placed in eight (8) different test tubes labeled A, B, C, D, E, F, G,
& H, respectively, and 4ml each of the following solvents; distilled water (H2O), ethyl ether,
concentrated & dilute hydrochloric acid (HCl), concentrated and dilute sulphuric acid(H2SO4), ethanol

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Int. J. Modern Chem. 2015, 7(1): 81-90 84

(C2H5OH), 10% sodium bicarbonate (NaHCO3) were added respectively and shake for 2 minutes and
warmed for 1 minute in hot water bath at 60oc.

2.8. pH Determination of the Dye

The dye extract (1g) was dissolved in distilled water (5ml) and pH meter was calibrated using
distilled water and inserted into the dye extract solution. Also, the coupled dye (1g) was dissolved in
distilled water (5ml) and pH meter was calibrated using distilled water and inserted into the coupled
dye solution.

2.9. Thin Layer Chromatography of the Dye Extract

The dye extract(1g) was dissolved in methanol (2ml) in a test tube and capillary tube was used
to stain the dye extract solution on chromatography plate (2cm x 10cm) and allowed to dry and was
placed in a mixture of methanol (3.5ml) & n-hexane (1.5ml) in chromatography tank.

3. Ultraviolet Spectroscopic Analysis

The ultraviolet spectroscopic analysis of the dye was carried out using a JENWAY 6305
spectrometer from the Nigerian Institute of Leather and Science Technology (NILEST), Zaria, to
obtain the wavelength of maximum absorption. The Spectrum of the dye is shown in Figure 7.

3.1. Dyeing of Chrome Tanned Leather with the Coupled Dye Extract

The chrome tanned leather (5g) was weighed and the coupled dye (0.25g) was weighed and
distilled water (4ml) was measured and boiled to 60oC and the chrome tanned leather was soaked in
cold water for 30 minutes then the dye was dissolved in warm water at 60oC.The wet chrome tanned
leather was placed in the dye solution in a conical flask and was agitated using a shaker for 30 minutes
then 1ml of formic acid was added into the mixture and agitated using a shaker for another 30 minutes
and the dye solution was decanted and the dyed leather was rinsed using cold water until there was no
visible colour change on addition of water and the dyed leather was placed on a white tile and allowed
to air dry at room temperature and the dyed leather was fastened for 24 hours on toggle frame using
toggle clips.

3.1.1. Dyeing of Cotton with the Coupled Dyed

The cotton fibre (2g) was soaked in warm water (60oC) for 2hours then 1ml of formic acid was
added into a beaker containing 10ml of water (60oC) and the dye (2g) was dissolved in the solution and
the wet cotton was added into the solution and was stirred regularly and kept on simmer for 1hour and
the cotton was removed and allowed to dry at room temperature.

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Int. J. Modern Chem. 2015, 7(1): 81-90 85

3.2. Assessment of Dyeing Property

3.2.1. Fastness of light (sunlight)

This test was carried out according to the official method of analysis by the society of Leather
Technologists and Chemists; A piece of dyed leather of size 3 x 3 cm was half covered with a black
polythene sheet such half of the length, 1.5 x 1.5 cm was half covered and the remaining half was left
uncovered exposed to daylight for 5 consecutive days between the hours of 9:00am – 3:00pm (6
hours); after which the change in color was compared to the uncovered and unexposed leather
respectively; using the standard grey scale.

3.2.2. Alkaline fastness

The leather 3cm X 3cm was dipped in sodium carbonate solution for 30 minutes, and dried at
room temperature without rinsing. The change in color was determined using the standard grey scale.

3.2.3. Acid fastness

A piece of dyed leather of size 3cm x 3cm, was immersed in 0.1M or 56% glacial acetic acid
solution for 30 minutes, and then allowed to dry at room temperature without rinsing. The color
change was assessed using the standard grey scale.

3.2.4. Wash fastness

The dyed leather 3cm x 3cm was dipped into a solution made by adding 5g (0.5%) of detergent
powder into 200cm3 of deionized water. This was placed in a water bath, and the temperature allowed
to rise to 40oC and was vigorously stirred for 30 minutes at 5 minutes interval. After 30 minutes, the
leather was placed in 100cm3 of distilled water at room temperature and allowed to stand undisturbed
for 1 minute and it was removed and gently squeezed by the hand. This washing and rinsing was
carried out 5 times and the leather was dried in the oven at 60oc.The change in the relevant surface of
the dyed leather was assessed by comparing it with unwashed leather, using the standard grey scale.

4. Results and Discussion

As presented in Table 1, it is possible to achieve a very soluble solution in both alkaline and
acidic medium except in ethyl ether which was partially soluble. The pH determination of the dye
extract and coupled dye is presented in table 2. The results prove that the dye is basic. Physical test of
the dye on acid, alkaline, light (sunlight) and wash fastness of the dyed cotton and leather in tables
4,5,6,7 respectively, showed good fastness property.
The percentage yield of the dye was calculated as follows:

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Int. J. Modern Chem. 2015, 7(1): 81-90 86

Percentage yield=

=0.928X100%
=92.89%

Table 1: The solubility test results

EXPERIMENT OBSERVATION INFERENCE
A Dye + distilled H2O Soluble with a light brown colour Readily soluble

B Dye + ethyl ether Two layer solution is formed Partially soluble

C Dye + Conc. HCl Soluble with dark orange colour Readily soluble

D Dye + 1M HCl Dark brown solution is formed with effervescence Readily soluble

E Dye + Conc. H2SO4 Dark brown solution is formed with effervescence Readily soluble

F Dye + 2M H2SO4 Brown solution is formed with no precipitate Soluble

G Dye + ethanol Light orange solution was formed with precipitate Soluble
H Dye + 10% NaHCO3 Light brown solution is formed Soluble

Table 2. Characterization of the extracted dye

SAMPLE pH TLC RF VALUE λmax(nm) COLOUR
DYE EXTRACT 9.0 Blue 0.83 480 Green
Green 0.86
Yellow 0.89
COUPLED DYE 8.2 Yellow 0.98 400 & 480 Brown
Orange 0.95

Table 3. The result of dyeing from coupled dye

EXPERIMENT RESULT AMOUNT OF DYE USED
Dye with chrome tanned Brown shade was obtained 5% of the dye
leather with partial fixation
Dye with cotton Pale brown shade was 2% of the dye
obtained with partial fixation

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Int. J. Modern Chem. 2015, 7(1): 81-90 87

Table 4. The result of acid fastness with coupled dye

DYED SAMPLE FASTNESS RATING
Chrome tanned leather 4
Cotton 3

Table 5. The result of alkaline fastness with coupled dye

DYED SAMPLE FASTNESS RATING
Chrome tanned leather 4
Cotton 4

Table 6. The result of sunlight fastness with coupled dye

DYED SAMPLE FASTNESS RATING
Chrome tanned leather 3
Cotton 3

Table 7. The result of wash fastness with coupled dye

DYED SAMPLE FASTNESS RATING
Chrome tanned leather 3
Cotton 2

Table 8. Key (interpretation of results fastness colour change)

GRAY SCALE RATING ASSESSMENT

5 Excellent
4 Very good
3 Good
2 Poor
1 Very poor

THIN LAYER CHROMATOGRAPHY OF DYE EXTRACT

Identification of component in chromatogram
Rf =

Dye Extract
For Blue
RF= = 0.83

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Int. J. Modern Chem. 2015, 7(1): 81-90 88

For Green
RF= = 0.86
For Yellow
RF= = 0.89
Coupled Dye
For Yellow
RF= =0.98
For Orange
RF= =0.95

Fig 1. Chrome tanned leather before dyeing Fig 2. Chrome tanned leather after dyeing

Fig 3. Toggling of chrome tanned leather after dyeing Fig 4. Cotton before dyeing

Fig 5. Cotton after dyeing Fig 6. Thin layer chromatography of dye

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Int. J. Modern Chem. 2015, 7(1): 81-90 89

Fig. 7. UV/Vis spectroscopy of coupled dye

5. Conclusion

The result obtained indicates that the dye extracted gave a good yield and was successfully
applied on leather, cotton, and wool. However, there was decrease in glossy appearance on the dyed
cotton and no colour change was observed with fastness property. The TLC showed that the dye
extract contained three components (blue, green and yellow) which prove that justicia carnea hooker
contains dyestuff. Also, the pH determination shows that the dye is basic.

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Int. J. Modern Chem. 2015, 7(1): 81-90 90

[4] Balter M. Clothes Make the (Hu) Man.Science, 2009, 325(5946):1329

[5] Belfer-cohen, A., Goring- Morris, A. N., Hovers, E..The dynamics of Pleistocene and early
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