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Henna extract: Can it be an alternative retanning agent?

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188
Henna Extract: Can it be an Alternative
Retanning Agent?
by
A.E Musa1, B. Madhan*, W. Madhulatha, S.Sadulla, G.A. Gasmelseed1
1
Department of Leather Technology, College of Applied and Industrial Science,
University of Juba, P.O.Box 321/1, Khartoum – Sudan
Central Leather Research Institute, Adyar, Chennai 600 020, INDIA
Abstract
Extract from the leaves of lawsonia inermis (henna),
widely distributed in Sudan, has been evaluated for
its utilization in the retanning of the leather and
presented in this paper. Leaves of henna have been
extracted for 1 hour with distilled water (1:10 w/v) at
temperature above 80˚C. The henna extract prepared
has been used for the retanning of wet blue leathers.
The effectiveness of henna extract in retanning of wet
blue leathers has been compared with wattle retanning.
The organoleptic properties of the leathers viz. softness,
fullness, grain smoothness, grain tightness (break),
general appearance, uniformity of dyeing of henna
retanned leather have been evaluated in comparison
with wattle retanned leathers. Henna retanning
resulted in leathers with good grain tightness. Dyeing
characteristics of henna retanned leathers have been
found to be better than wattle retanned leathers.
Also physical strength characteristic and shrinkage
temperature and economic viability were noted. The
effluent arising from this retanning system has been
analyzed for its environmental impact.
Resumen
Extractos de las hojas de lawsonia inermes (alheña),
por doquier distribuidas en El Sudán, se han evaluado
para su utilización en el recurtido del cuero y
presentado en esta publicación. Hojas de alheña
fueron tratadas por una hora con agua destilada (1/10
peso/volumen) a una temperatura superior a 80˚C.
El extracto de alheña así preparado se ha utilizado
para recurtir cueros curtidos al cromo. La efectividad
el extracto de alheña es comparable con recurtidos
con mimosa. Las propiedades de toque de mano, v.
y g. Blandura, llenura, finura de flor, firmeza de flor
(quiebre), apariencia general, uniformidad del teñido
de cuero recurtido por alheña han sido evaluadas
en comparación con cueros recurtidos con mimosa.
También las características de resistencia física y
temperatura de contracción y viabilidad económica
* Corresponding Author - e-mail address: bmadhan76@yahoo.co.in .
Manuscript received March 22, 2007, accepted for publication December 4, 2007
JALCA, VOL. 103, 2008
fueron examinadas. El efluente resultante de este
sistema de recurtido ha sido analizado por su impacto
medioambiental.
Introduction
Lawsonia inermis is a member of the family Lythraceae
cultivated in many tropical and warm temperate regions as a
hedge plant. Large scale cultivation for the sake of the leaves,
which yield dye, is confined to India, Egypt and Sudan and
to some extent, Madagascar, Pakistan and Australia.1 Henna
leaves are commonly used as cosmetics for staining hands
and feet in northern Nigeria and an ingredient in local
medicinal preparations in the Middle East and Asia. The
aqueous extract of leaves of Lawsonia inermis has been shown
to possess reproducible activity in vitro against a wide variety
of microorganisms.2,3 The chemistry of the constituents of
Lawsonia inermis has been of interest for many researchers
and the occurrence of β- sistosterol glucoside,4 flavonoid,5
quinoids,6 naphthalene derivatives,7 gallic acid,6 coumarins,8
and xanthones,9 luteolin,4 and phenolic glycosides lawsoniaside
and laioside in the Lawsonia leaves has been reported.10
Analysis of air- dried leaf powder gave the following average
values: moisture 8.97%, ash 14.85%, tannin 10.2%, and water
– soluble matter 25- 33%. Aqueous solutions are orange in
colour and show green fluorescence. The principal colouring
matter is lawsone, 2-hydroxy 1,4 naphthaquinone (C10 H6 O3
m.p 190 0C ) which is present in dried leaves in concentration
of 1.0 – 1.4% . Beside lawsone, other constituents present
in henna are gallic acid, glucose, mannitol, fats, resins (2%),
mucilage and traces of an alkaloid1. Gupta et al reported
the isolation of a second naphthaquine beside lawsone is
termed isoplumbagin11 (Figure 1), (2-methyl-6-hydroxy-1,4-
naphthaquinone C11H8O3 mp 67-68 0C) which has been
extracted from the stem bark of lawsonia. Afzal et al reported
four flavonoid glucosides (Figure 2) from the leaves of lawsonia
inermis5. They have been identified as apigenin-7-glucoside,
apigenin-4/-glucoside, luteolin, luteolin-7-glucoside, luteolin-
3/-glucoside and Acacetin-7-glucoside.
 Henna Extract: Can it be an Alternative Retanning Agent? 189

Table I
Formulation of post tanning process
Raw material: Shaved wet blue leathers (cow) of thickness ~1.2 mm .
% chemicals for post tanning process is based on shaved weight
Process % Product Duration Remarks
Neutralization 100 Water
1 Sodium formate
0.75 Sodium bicarbonate 3 x 10/ + 60 min pH 5-5.5
Retanning 15 Henna (Experimental)/ 1 hour
Wattle (Control)
Fatliquoring 5 Lipoderm liquor SAF 45 min
(Syntheic fatliquor)
Dyeing 3 Acid black dye 45 min Penetration of .
dye was checked
Fatliquoring 5 Lipoderm liquor SAF 45 min
(Syntheic fatliquor)
Fixing 1.5 Formic acid 3 x 10 +30 min pH 3.5
Washing 200 Water 10 min Leathers were piled over
night; Next day set,
hooked to dry, staked,
trimmed and buffed

Apigenin – 7- glucoside R1 = H ; R2 = glucose

Apigenin – 4/- glucoside R1 = glucose ; R2 =H

a b
Figure 1: Quinones as secondary metabolites isolated from Lawsonia .
inermis a) Lawsone and b) Isoplumbagin

Luteolin R1 = R2 = H
Henna contains 5% to 10% gallic acid and tannin.12 Also Luteolin – 3/- glucoside R1 = glucose ; R2 =H
one compound based on 5- alloxy- 7- hydroxycoumarin was Luteolin -7- glucoside R1 = H; R2 = glucose
isolated from the whole extract of lawsonia inermis.13 Other
constituents present in henna are resin (2%), mucilage and Figure 2: Flavonoids as secondary metabolites isolated .
traces of alkaloids1. The flowers of henna plant have a strong from Lawsonia inermis
aroma and yield, on steam distillation, 0.01% - 0.02% of an
essential oil, with brown and dark brown color and a strong
fragrance1.
Experimental
Materials
Extracts of henna had been shown to contain anti-fungal and Conventionally processed wet blue cow sides were taken for
anti-bacterial characteristics.14,15 Henna finds use in traditional the tanning trials. Henna leaves were sourced from Sudan.
medicinal preparations15 and in textile industry as a dyeing.16 Chemicals used for post tanning were of commercial grade.
There are no reports available on the use of henna in leather. Chemicals used for the analysis of spent liquor were of
Since the henna extract contains mixture of several compounds analytical reagent.
with varied molecular weight including polyphenols, an
attempt has been made in this study to utilize them for the
retanning of wet blue leathers.

JALCA, VOL. 103, 2008

 Henna Extract: Can it be an Alternative Retanning Agent?
Table II
Shrinkage temperature of crust leathers
retanned with henna and wattle
Sample Shrinkage temperature, Ts (˚C)
Wattle (Control) 123±3
Henna (Experimental) 121±2
Note-Shrinkage temperature of wet blue .
leathers were 109±2˚C
Table III
Organoleptic properties of crust leathers
retanned with henna and wattle
Property Henna Wattle
(Experimental) (Control)
Fullness 8±0 7.33±1
Grain tightness 8.5±0.4 6.7±0.2
Roundness 8.5±0.4 7.5±0
Grain smoothness 7.7±0.5 7.7±0.5
Softness 6.2±0.2 7±0
General appearance 8.3±0.5 7.5±0.4
Aqueous Extraction of Henna Leaves
The required amount of ground henna leaves(dried) were
soaked in water (1:10 w/v) at temperature above 80 0C in water
bath for an hour, filtered through the a piece of cotton cloth
and the volume of the henna extract is noted. Part of the henna
extract was filtered through Whatman no.1 filter paper and 10
mL of filtrate were used for the determination of percentage
total solubles.
Retanning Trials
Two wet blue cow hides were taken. 2 sq. ft of leather in the
official sampling portion (butt region) of the two left sides were
taken for experimental retanning trails using henna extracts.
Similarly 2 sq. ft of the corresponding two right halves were
taken for the retanning using wattle as a matched pair control
as a comparison for the experimental leathers. The post tanning
process mentioned in Table 1 is followed for both experimental
and control leathers.
Determination of shrinkage temperature:
The shrinkage temperature of both control and experimental
retanned leathers were determined using the Theis shrinkage
tester.17 A 2 cm sample, cut out from the leather was clamped
between the jaws of the clamp, which in turn was immersed in
a solution of glycerol: water mixture (3:1). The solution was
stirred using mechanical stirrer attached with the shrinkage
tester. The temperature of the solution was gradually increased
and the temperature at which the sample shrinks was noted.
190
Table IV
Visual evaluation of the dyeing
characteristics of crust leathers retanned
with henna and wattle
Property Henna Wattle
(Experimental) (Control)
Uniformity of dye Good Good
Shade intensity Very Good Good
Differential Dyeing Nil Nil
Visual assessment of the crust leather:
Experimental and control crust leathers were assessed for
softness, fullness, grain smoothness, grain tightness (break),
general appearance by hand and visual examination. Three
experienced tanners rated the leathers on a scale of 0-10 points
for each functional property, where higher points indicate
better property. The tanners have also evaluated the dyeing
characteristics viz., uniformity of dye, shade intensity and
differential dyeing for both experimental and control crust
leathers.
Physical testing
Samples for various physical tests from experimental and
control crust leathers were obtained as per IULTCS methods.18
Specimens were conditioned at 20±2 0C and 65±2% R.H over
a period of 48 hrs. Physical properties such as tensile strength,
percentage elongation at break,19 grain crack strength20 and tear
strength21 were measured as per standard procedures. Each
value reported is an average of four (1 along the backbone, 1
across the back bone from each side of the two sides) samples.
Measurement of leather Softness
Softness measurement of experimental and control crust
leather was carried out as per standard method.22 Samples were
conditioned at 20±2 0C and 65±2 % R.H over a period of 48
hrs before the measurement. Circular aperture of diameter 35
mm is used for the softness measurement.
Scanning Electron Microscopic Analysis of Leather Samples:
Samples from experimental and control crust leathers were cut
from official sampling position. Samples were directly cut into
specimens with uniform thickness without any pretreatment.
All specimens were then coated with gold using Edwards E306
sputter coater. A Leica Cambridge Stereoscan 440 Scanning
electron microscope was used for the analysis. The micrographs
for the grain surface and cross section were obtained by
operating the SEM at an accelerating voltage of 20 KV with
different lower and higher magnification levels.
Analysis of spent liquor
The spent liquor from control and experimental post tanning
processing were collected, filtered and analyzed for chemical
oxygen demand (COD), Biochemical oxygen demand (BOD5),
and total solids (TS) as per standard procedures.23
JALCA, VOL. 103, 2008
 Henna Extract: Can it be an Alternative Retanning Agent? 191

Table V
Physical strength characteristics of crust leather retanned using henna (Exp) and wattle (Con.)
Parameter Henna Wattle BIS norms*
Tensile strength (Kg/cm2) 252.32±16.8 250.92±20.9 250
Elongation at break (%) 60.15± 9.48 64.58±3.84 60-70
Tear strength (Kg/cm thickness) 39.93±7.9 42.37±3.58 30
Load at grain crack (kg) 24±4 26±6 20
Distention at grain crack (mm) 10.64±0.72 11.60±0.4 Min 7
*-Bureau of Indian standards (BIS) specification for chrome retanned upper leathers

Table VI Table VII

Softness test of the crust leather from
cow wet blue retanned with henna extract
(Exp) and Mimosa (Con.)
Leather Softness Value
Henna (Experimental) 4.72±0.12
Wattle (Control) 5.53±0.23
Results and Discussion
Shrinkage temperature
The shrinkage temperature of wet blue crust leathers retanned
using henna and wattle is given in Table II. The wet blue
leathers resulted in shrinkage temperature of 109˚C, however
the retanning with wattle and henna resulted in increase of
shrinkage temperature to 123˚C and 121˚C respectively. It
is clear that the treatment of henna enhances the shrinkage
temperature significantly similar to the case of wattle; hence
retanning with henna appears to be a promising option in
terms of its reactivity with the leather matrix.
Characteristic of spent liquor for control
and experimental post tanning trials
Parameter Wattle Henna
(Control) (Experimental)
COD (mg/l) 92960±3500 79680±1260
BOD5 (mg/l) 33000±900 30000±850
Total solid (mg/l) 22420±840 31760±860
leathers have been evaluated by experienced tanners and the
results are given in Table IV. Experimental henna and control
wattle retanning have been found to result in leathers with
good uniformity in color. The shade intensity of the henna
retanned leathers has been found to be better than the wattle
retanned leathers. No differential dyeing (between grain and
flesh) has been observed for both henna and wattle retanned
leathers. It is clear that the use of henna did not affect the
dyeing characteristics of the leather compared to control;
rather it enhances the shade intensity of the leathers, which is
benevolent in obtaining leathers with brilliant shades.

Organoleptic properties of henna retanned leathers Physical strength characteristics

The organoleptic properties of leathers retanned using henna
and control wattle is given in Table III. From the table it
is observed that retanning with henna resulted in leathers
with good grain tightness and roundness compared to wattle
retanned leathers. The fullness of the leathers with henna
retanning had been found to be comparable to that of wattle.
However, the softness of leathers with wattle retanning is found
to be better than that of henna. To be an effective agent for
retanning, the retanning material should improve the fullness,
grain tightness and roundness of the leather, as they are the
important parameters especially for making upper leathers. The
grain smoothness of henna retanned leathers has been found
to be similar to that of wattle retanning. On the whole the
leathers retanned with henna had been found to be better than
wattle retannng. Hence use of henna for retanning appears to
be a fruitful option for making leathers with good organoleptic
properties.
Dyeing Characteristics of Henna Retanned Leathers
The dyeing characteristics of henna and wattle retanned
of henna retanned leathers
The physical strength measurements of matched pair henna
retanned experimental and wattle retanned control leathers are
given in Table V. The physical strength measurements viz.,
tensile strength, elongation, tear strength, load at grain crack
and distension at grain has been found to be comparable. The
strength values of henna retanned leathers have been found to
meet the BIS standards24 for chrome retanned leathers. The
softness values for the experimental and control leathers are
given in Table VI. It is seen that the softness of wattle retanned
leathers are better than that of the henna retanned leathers. The
values are coinciding with the softness measurements evaluated
by the subject analysis given in Table III.
Scanning Electron Micrograph Analysis of Leathers
The scanning electron micrograph pictures (grain and cross
section) of wattle and henna retanned leathers are shown in
Figures 3a to d. The grain structure of wattle (Fig. 3a) and
henna (Fig. 3c) retanned leathers appear almost similar. The
grain corium junction of the cross section of henna retanned
JALCA, VOL. 103, 2008
 Henna Extract: Can it be an Alternative Retanning Agent? 192

a b

c d
Figure 3: Scanning Electron Micrograph of a) Grain (X150) of wattle retanned leather b) Cross section (X100) of wattle retanned leather .
c) Grain (X100) of henna retanned leather and d) Cross section (X100) of henna retanned leather

leathers shown in Fig. 3d appears to be more compact than the
cross section of wattle retanned leathers (Fig. 3b). The picture
correlates well with the organoleptic properties assessment,
which exhibited the grain tightness and roundness of the henna
retanned leather better than the wattle retanned leathers.
Spent liquor Analysis
The COD, BOD5 and TS of the spent liquor for both
experimental and control trials were determined and are given
in Table VII. From the table it is observed that the COD and
BOD of the spent liquor processed using henna retanning is
lesser than the spent liquor from wattle retanning. However
the solid content of henna retan liquor has been observed to
be higher than the wattle retan liquor. Even though the solid
content of the henna retan liquor is higher, the degradability of
the same is easier than the wattle retan liquor.
used for leather making is around 1.75 US$. Therefore the use
of henna for retanning certainly has commercial advantage.
Conclusions
Most organoleptic properties of the experimental leathers
produced from henna leaves extract are better than control
leathers produced from wattle. However softness property is
better in the case of wattle retanned leather and the physical
strength properties are comparable with the matched pair
control leathers. Retanning with henna also facilitates in intense
dyeing. Hence using henna appears to be a good alternative for
the retanning processes. Apart from being technically feasible,
retanning with henna is also economically viable as the cost of
the henna extract is cheaper. Further exploration is required to
find effective utilization of henna extract in leather processing.

Economic viability of using henna for retanning

Any development of a new process requires commercial
feasibility, followed by cost effectiveness. The annual production
of henna dried leaves in Sudan is estimated at 2925 tons and
the price per ton of henna is around 500 US$. Total soluble of
henna leaves 27-33 %. Hence cost per kg of henna extract will
be around 1.5 US$, where as the cost of per kg of wattle extract

JALCA, VOL. 103, 2008

 Henna Extract: Can it be an Alternative Retanning Agent?
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