International Journal of Advanced Research and Publications

ISSN: 2456-9992

Comparative Studies On Graham Glass Condensing

Model Types “As” And “Bs” For Extraction Of
Natural Dyes From Lawsonia Inermis
Jekada J.Z., Gonah C. M.,, Garkida A. D.,, Ladam Z
Nigerian Institute of Leather and Science Technology, Samaru- Zaria. 07031002880
jekadajuliuszachariah@gmal.com, jekadaj24@yahoo.com

Department of Science Technology Ahmadu Bello University Zaria. Department of Glass and Silicate Technology, 08036980601
Nomhat2003@gmail.com

Ahmadu Bello University Zaria. Department of Glass and Silicate Technology,08034522439

adelezik@yahoo.com

Kaduna State University, Kaduna. Department of Chemistry.07030475898

ladanzakari@gmail.com

Abstract: This study was undertaken with a view to investigating the effect of the number of bulbs on the performance Graham outer
jacket glass condensers. AutoCAD was used to design Graham condensers varying the number of bulbs from one to ten (1-10) on the outer
jacket; while maintaining the following specifications: outer bulbs size of θ48 mm, distance from bulb to bulb 18mm,inner tube length θ
9/679 mm, outer tube length θ 40/720, outlets and inlets θ 9/1.5 mm and the length of quick fit 84 mm. Ten (10) assorted pieces of each type
“As” and “Bs” of this modified structures of Graham condensing models were fabricated. For types “As” Graham condensers, the outlet and
inlet tubes were joined to their jackets while for the type “Bs” Graham models, the outlet and the inlet tubes were joined directly to their
inner tubes. The performance of these condensers were evaluated using extraction protocol involving leave of lawsonia inermis (natural
dye) acetone used as solvent. Results of extraction obtained showed types “As”Graham condensing models gave the highest yield of crude
extracts of 43.00% and types “Bs” condensing models with 7 bulbs yielded 41.35%.

Keywords: Graham Condenser, Extraction and Lawsonia Inermis

1.1 Introduction
Condensers are devices designed to separate one or more
components of a vapour mixture by reducing the gaseous
vapour to its liquid form; this condensers uses the
principle of heat transfer. A heat exchanger is a device
that is used to transfer thermal energy (enthalpy) between
two or more fluids, (from one medium to another), or
between solid surface and a fluid, or between solid
particulates and a fluid, at different temperatures and
thermal contact. In heat exchangers, there are usually no
external heat and work interactions [1][2]. The science of
heat transfer predicts that energy transfer which takes
place between material bodies as a result of temperature
gradient is known as thermodynamics. One of the most
important fields of thermodynamics is heat transfer which
relates to transfer of heat between two media. The concept
of heat transfer is used in a wide range of devices like
heat exchangers, evaporators, condensers, radiators,
coolers and heaters. Thermodynamics also involves the
study of various types of power plants like thermal plants,
nuclear power plants, hydroelectric power plants based on
renewable energy sources like solar, wind, geothermal and
water waves[1][3][4]. Graham condenser (also Grahams
or Inland Revenue condenser) has a coolant-jacketed
spiral coil running the length of the condenser serving as
the vapour/condensate path. This is not to be confused
with the "coil condenser". The coiled condenser tubes
inside will provide more surface area for cooling and for
this reason it is most favourable to use but the drawback
of this condenser is that as the vapours get condensed, it
tends to move them up in the tube to evaporate which will
also lead to the flooding of solution mixture. The Graham
Condenser consists of an inner coil surrounded by an outer
tube. The coolant flows through the outer tube and the
substance condenses inside the inner coil. Graham
Condensers should not be confused with Coil Condensers
[5]. It has been suggested that Graham Condensers are
useless they cannot be used for normal distillations
because the condensed liquid doesn’t flow to the receiving
flask, ending up “clogging” the path. The pressure starts to
rise in the apparatus, trying to push the liquid forward; this
might make joints pop off or other sort of damage, they
can’t be used in refluxes or either position due to the
narrow path of the inner coil, pressure rises too much and
vapour starts shooting out from the top of the condenser.
The only time they can actually be useful is in distillations
where the condenser is held vertically [6][7]. The Graham
Glass condenser consist of outer glass tube usually has
two hose connections, and a coolants (usually tap water or
chilled water/antifreeze mixture) is passed through it. For
maximum efficiency, and to maintain a smooth and
correctly directed thermal gradient so as to minimise the
risk of thermal shock to adjacent glassware, the coolant
usually enters through the lower fitting and exists through
the higher fitting. Maintaining a correct thermal gradient
(entering coolant at the cooler point) is the critical factor.
Multiple condensers may be connected in series. Normally
a high flow rate is not necessary to maintain a cooling
surface [8][4].

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 International Journal of Advanced Research and Publications
ISSN: 2456-9992
1.2 Extraction
Frequently, organic chemists must separate an organic
compound from a mixture of compounds, often derived
from natural sources or products of synthetic reactions.
One technique used to separate the mixture compounds is
called extraction. Extraction is a process that selectively
dissolves one or more of the mixture components into an
appropriate solvent. The solution of these dissolved
compounds is often referred to as the extract. Extraction
process include removal of soluble compounds from a
solid matrix, such as in the brewing of coffee or tea, or in
decaffeinating coffee with liquid carbon dioxide. In the
organic chemistry laboratory, however, extraction almost
always refers to the transfer of compounds from one liquid
solvent to another [9].
3 Solvent Extraction
Nature rarely provides a raw materials in a pure form and
in a few processes produce pure products. Because of this
thoughtless provision of nature and the ineptitude of
chemical synthesis, physical separation has become the
most important single industrial process, the petroleum,
chemical, and petrochemical industries, in general, have
large investments in separation equipment and spent even
more in operation. The more complicated our industrial
economics becomes, the more different are the material
required in a relative pure form for feedstock, and the
more finished from by-products and impurities [10]. In
definition, separations considered here are those
separations where mixtures are divided into two pure
compounds or at least into two or more fractions having
different compositions by processes sometimes classified
as “diffusional or mass transfer” operation. Common
amount these processes are fractional distillation,
fractional crystallization, adsorption, evaporation,
absorption and solvent extraction [11]. A compound can
be separated from impurities in a solution by extracting
the compound from the original solvent into a second
solvent. For the process to be selective, the compound
must be more soluble in the second solvent than in the
first solvent. Additionally, the two selected solvents must
be immiscible, or not soluble in one another, so that they
produce two separated solvent layers. After dissolving the
mixture in the first solvent, the solution is added to a
second solvent. The two layers are vigorously mixed to
maximize the surface area between them. This mixing
facilitates the transfer of a dissolved compound from one
solvent layer to another. Once the transfer process is
complete, the layers are allowed to form again [12][10].
1.4 Natural dyes
Natural dyes are dyes or colorants derived from plants
invertebrates or minerals. The majority of natural dye are
vegetable dye from plant sources, roots, berries bark
leaves and woods; and other organic sources such as fungi
and lichens. Natural dyes are friendly and convenient to
use. They are familiar sources that can spark creative
ideas and widen ones view of the world in experimenting
with them. Colours can be coaxed from all kinds of
natural sources. It is important to note that all natural dye
recipes are safe and non-toxic [13][14]
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2.0 METHODOLOGY
2.1 Design of Condensers
According to [15]. Proper design or selection of
condensers are very important factors for satisfactory
performance of cooling systems which is based on the
industrial design principles. Conventionally, the design
and lengths specification for glass condensers in practice
range from 120mm to 600mm [16]. AutoCAD was used
to design Graham condensers by varying the number of
bulbs from one to ten (1-10) on the outer jacket; while
keeping the lengths (720mm) constant. Ten (10) pieces of
types “As” and “Bs” of this modified structures of
Graham condensers were fabricated with quick-fit and
their accessories (type “As” conventional and type “Bs”
unconventional). For types “As” Graham condensers, the
outlets and inlet tubes were joined to their jackets while
for the types “Bs” Graham models, the outlet and the inlet
tubes were joined directly to their inner tubes. The
difference in design and operation of types “As” Graham
condensers and types “Bs” Graham condensers is the
coolant flow in the outer tube for the types Graham
condensers while for type “Bs”, the coolant flows in the
inner tubes [4]. Fabrication was done at Scientific
Equipment Development Institute (SEDI). Minna, Niger
State Nigeria. Standard method of scientific glass
technology fabrication of condensers was adopted used
suitable tools [17].
2.2 Fabrication of Graham Condensing Models
About 48” length of 6mm diameter glass tubing and
mandrel covered with ceramic paper are essential for the
coil winding. The mandrel was preheated slightly and the
hook was bent on the end of the 6mm tube. The hook was
knit to the rod attachment on the mandrel. The 6mm glass
tubing was heated in a large bushy flame until it reaches
working temperature to be bend and coiled while the
spacing was carefully observed. The hook end of the coil
was broken away from the mandrel as soon as the coil and
mandrel were cooled. The glass coil was removed from
the mandrel while synchronizing the rotation and running
them under cool tap water. The ends of the coil were cut,
fire polished and flame annealed. The same principles of
blowing bulbs was employed in blowing of the bulbs on
the outer jacket for the twenty assorted pieces of types
“As” and “Bs” of condensing models. The performance of
these condensers was evaluated using industrial acetone
grade (CH3COCH3) for extraction of natural dye from
Lawsonia inermis (lallebature) plant leaves with voucher
number 3004 which was identified in the Herbarium unit
of Department of Biological Sciences , ABU, Zaria,
Kaduna State.
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 International Journal of Advanced Research and Publications
ISSN: 2456-9992

in series to the outlet tube for the four extraction set-up.

Heat was supplied from four electric heating mantles and
regulated at a constant temperature of 56°C to that of the
boiling point of the organic solvent 56˚C. The extract
continued to siphon into the reservoirs for six hours till the
solvent in the soxhlet extractor chambers was colourless
from the initial green colour. Extraction is said to be
completed when the solvent in the Soxhlet extractor is
colourless [19][12]. The flasks were rinsed properly with
fresh acetone then transferred from the reservoirs into
collecting sample bottles placed on top of water bath set at
50oC below the boiling point of the solvent. This was
allowed to evaporate the remaining solvent leaving only
the crude extract which was weighed using analytical
Plate I: Samples of type “As” Graham Condenser balance.
(conventional)
2.4 Results of Extraction
Bar charts Figures 1-3 showed the performances of
individual condensing models of both types “As” and
“Bs” of Grahams. Whereby TAG type “As” Graham, TBG
type “Bs” Graham.

Plate II: Samples of type “Bs” Graham Condenser

(unconventional)

Characterization of the Condensers

Soxhlet extraction method EPA 2701C [18].was adopted
for the extraction of natural dye from Lawsonia inermis
(Lallebature) plant leaves at the research Laboratory of
Glass and Silicate Technology Department of Ahmadu
Bello University, Samaru, Zaria.

2.3 Extraction of natural dye

The modified Graham condensing models were used to
carry out solvent extraction of Lawsonia inermis
(lallebature) plant leaves. The leave was washed with
water to removed dirt and other adhering materials, then
dried in a tray drier at 40˚C for 48 hours and finely ground
with the help of a grinding machine. 20g of the ground
Lawsonia inermis (lallebature) was wrapped in thimble,
placed inside 500ml soxhlet extractors. The four soxhlet
extractors were fitted or connected with four 500ml round
bottom flasks which served as the reservoir for the
concentration. About 300ml of the solvent (acetone) was
poured through the soxhlet opening to allow the samples
and the solvent to saturate in the extracting chamber. The
four sets of the condensers were connected vertically
under reflux position at 50°C and operated concurrently,
the temperature was allowed to gradually build up to
boiling point of the organic solvent and extraction time of
6 hours was set for all the samples. Acetone was used as
the organic solvent and water as the coolant flowed
through the hose which was connected from the water
source to the inlet tube; and another hose was connected

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 International Journal of Advanced Research and Publications
ISSN: 2456-9992
2.5 RESULT AND DISCUSSION
Percentage yield of extraction
Graham condensing models “As” and “Bs” show
percentage yields of the crude extracts at different number
of bulbs from 1-10. Graham condensing models, type
“As’’ presented in Figure 1 with 7 bulbs gave 43.00%
yields of extract followed by condensing model with 4
bulbs 37.90% while the lowest percentage of extract with
32.05% was observed in condensing model with 1 bulb.
This abnormal behaviour observed in condensing model
with one bulb might have resulted from the prolonged
contact with the coolant which is in agreement with [6]. In
Figure 2 of Graham types “Bs” condenser with 7 bulbs
gave the highest percentage of extracts 41.35% followed
by condensing model with 10 bulbs yield of 39.60% and
the least yield of crude extracts was obtained with
condensing model with one bulb 33.95% which is in
conformity with the results obtained in types “As”
Graham condensing model with one bulb. With the
modification of Graham condensing models by
introduction of bulbs at the outer jacket which increases
the surface area of the condensers, it was generally
observed that it disagree with the finding of [6][7]. that it
cannot be used in refluxes due to the narrow path of the
inner coil. Figure 3 shows the overall performance of the
models which established their effectiveness and optimum
extraction, which was found on the condensing models
with numbers of 7 bulbs with the highest yields of crude
extracts. Further fabricating of these condensing models
with bulbs above or below 7 will amount to waste of
production, cost, materials and time.
2.6 Conclusion
The following conclusions are drawn from many other
factors that might have affected the results in one way or
the other such as inaccurate constructions of the
condensers since these were manually fabricated. Twenty
assorted types “As” (conventional) and “Bs”
(unconventional) Graham condensing models were
designed and fabricated. The efficacy of these condensers
was established using extraction of natural dyes from
lawsonia inermis (lallebature) plant leaves. The highest
yield of crude extracts was obtained in Graham
condensing models with 7 bulbs in both types “As” and
“Bs” with 43.00% and 41.35% yields respectively.
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