See discussions, stats, and author profiles for this publication at: https://www.researchgate.

net/publication/362417775

Investigation of geranium oil extraction performance by using soxhlet

extraction

Article in Materials Today Proceedings · August 2022

DOI: 10.1016/j.matpr.2022.07.276

CITATIONS READS

10 2,277

6 authors, including:

Rajesh Yennam
Hpcl green R&D Center at Bangalore and KKWIEER
19 PUBLICATIONS 95 CITATIONS

SEE PROFILE

All content following this page was uploaded by Rajesh Yennam on 02 August 2022.

The user has requested enhancement of the downloaded file.

 Materials Today: Proceedings xxx (xxxx) xxx

Contents lists available at ScienceDirect

Materials Today: Proceedings

journal homepage: www.elsevier.com/locate/matpr

Investigation of geranium oil extraction performance by using soxhlet

extraction
Yennam Rajesh a,⇑, Nabeel M. Khan a, Abdul Raziq Shaikh a, Venkat S. Mane a, Gaurav Daware a,
Ganesh Dabhade b
a
Department of Chemical Engineering, K. K. Wagh I. E. E. and R Nasik (Affiliated to S. P. Pune University), MS 422003, India
b
Department of Applied Science, K. K. Wagh I. E. E. and R Nasik (Affiliated to S. P. Pune University), MS 422003, India

a r t i c l e i n f o a b s t r a c t

Article history: Geranium oil (Pelargonium graveolens) is widely used as main ingredient in the production of perfumes
Available online xxxx as well as cosmetics etc. The essential oil is also used in aromatherapy treatment in various health issues
occurred in rural areas. In literature, several authors are used the different traditional extraction meth-
Keywords: ods; such as steam distillation, hydro distillation and solvent extraction etc. In this work, author used
Geranium Leaves the novel technique as soxhlet extraction of geranium oil extraction. The purpose of this work is to inves-
Soxhlet Extraction tigate the suitable method for getting the higher yield with lower cost and limited facilities. To investi-
Organic Solvents
gated the performance of soxhlet extraction technique by using different organic solvents like n-Hexane,
Steam Distillation
Methanol, Chloroform, Toluene and Water. Among all the solvents, n-Hexane and Toluene are provided
the satisfactory results with soxhlet extraction of geranium oil yield as 0.08–0.1 %. The operating condi-
tions of soxhlet extraction as Temperature (60–12 °C) and time (120–240 min). Also, the author calcu-
lated the Mass & Energy balances of soxhlet extraction are 6 (V/W) and 75 KW-Hr, whereas for steam
distillation Mass & Energy balances are 0.5 (V/W) and 42 KW-Hr. Even though the yield is small compared
to steam distillation, but this work will be applicable for lab scale extraction of geranium oil as well as
essential oils with lower cost.
Copyright Ó 2023 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the Advances in Chemical
Engineering and Science.

1. Introduction to geranium surely help the patient cope with the discomfort. This has been
employed as a flavouring agent in food as well as alcoholic and
Geranium (Pelargonium graveolens) is a member of the Gerani- non-alcoholic beverages. It works as an insect repellent [1]. Gera-
aceae family. A perennial hairy shrub native to South Africa that nium oil, one of the best natural perfumes, is commonly used in
grows up to one metre in height and is also grown in India, France, soaps and detergents since its unique character is never challenged
Italy, Spain, Central America, Egypt, Japan, and the Congo. The by the alkalinity of soaps. In aromatherapy applications, geranium
chemical ingredients of its essential oil are eugenol, geraniol, essential oil relieves stress, anxiety, melancholy, weariness, and
citronellol, geraniol, linalool, citronellyl formate, citral, myrtenol, tension, increases attention, improves cognitive function, and bal-
terpineol, methone, and sabinene. It was used to treat dermatitis, ances emotions and hormones [2]. Furthermore, this oil is becom-
eczema, aged skin, certain fungal infections, and anxiety and stress. ing increasingly popular as an anti-diabetic, anti-cancer,
The oil has antibacterial properties and is a significant component antibacterial, and antimicrobial agent.
in the treatment of endometriosis. This oil is also used for its calm- Geranium (Fig. 1) was first introduced to India in the nineteenth
ing characteristics, as a nerve tonic, to treat throat infections, to century in the southern climate, and it now grows throughout the
treat blood disorders, diabetes, and menopausal difficulties. country. Pelargonium
hortorum and Pelargonium graveolens,
There have been some accounts of it being used as a supportive for example, are planted as attractive plants in gardens and parks
therapy in the treatment of uterine and breast cancer, and it can to produce a pleasant smell. Zonen geranium (Pelargonium
hor
torum), fragrant geranium (Pelargonium sp.), regal pelargonium
⇑ Corresponding author. (Pelargonium
domesticum), and royal ivy geranium (Pelargo-
E-mail address: [email protected] (Y. Rajesh). nium peltatum) are the four commercial geranium species [3].

https://doi.org/10.1016/j.matpr.2022.07.276
2214-7853/Copyright Ó 2023 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the Advances in Chemical Engineering and Science.

Please cite this article as: Y. Rajesh, N.M. Khan, A. Raziq Shaikh et al., Investigation of geranium oil extraction performance by using soxhlet extraction,
Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2022.07.276
Y. Rajesh, N.M. Khan, A. Raziq Shaikh et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 1. Geranium Plant.

Geranium oil is one of the most valuable natural resources for combination of reflux boiling and Soxhlet extraction (both assisted
the perfumery and cosmetic sectors since it is commonly utilised by electrical heating) to perform two extraction steps (boiling and
as a floral substitute for the rose aroma. Geranium oil continues rinsing), followed by extractant recovery. Ultrasound-assisted
to be an intriguing natural substance, as evidenced by recent Soxhlet extraction in which an extractor based on Soxhlet’s physi-
papers. Geranium oil has a floral rosy aroma with green herbal cal–chemical principles that took advantage of ultrasound effects
fresh minty earthy characteristics and is used in high-end per- to extract total fat from oil seeds like sunflower, rape, and soy-
fumes. It is frequently utilised as a heart note in masculine per- abean [6].
fumes, lending a flowery flavour to green and fougere In Conventional Soxhlet extraction, Thermal breakdown of ther-
compositions. Geranium oil is made by distilling the green foliage molabile target species can occur when samples are extracted at
of Pelargonium graveolens or some of its hybrids, as well as the the solvent boiling point for long periods of time. A traditional
flowers (which are quite fragrant). This aromatic plant is widely Soxhlet apparatus also lacks agitation, which could assist speed
grown in Reunion Island (Bourbon type), Madagascar, Egypt (North up the process. In Automated Soxhlet extraction, the Soxtec coun-
African type), China, and, more recently, India. Steam distillation is terpart B811 extractor, able to perform the same steps as a Soxtec
currently the only industrial method for extracting geranium oil. device, emerged to implement the possibility to operate also as a
This process is inefficient, and key oil components are thermally conventional Soxhlet apparatus. The overall performance of the
degraded due to the high temperatures required (more than B811 extractor is computer-controlled. And in Ultrasound-
100 °C) [4]. assisted Soxhlet extraction, the use of ultrasound on the sample
Soxhlet Extraction is a time-honored method in which a sample cartridge produces results that are comparable to, if not better
is placed in a thimble holder and progressively filled with con- than, those achieved by traditional Soxhlet leaching (official ISO
densed fresh extractant (the solvent used for extraction) from a method); nonetheless, it significantly reduces the number of Soxh-
distillation flask. A syphon aspirates the solute from the thimble- let cycles required in the traditional procedure [7].
holder and unloads it back into the distillation flask when the liq- Microwave assisted Soxhlet Extraction is the most successful
uid reaches the overflow level, transferring the extracted analytes endeavour to improve Soxhlet performance using microwaves,
into the bulk liquid. This procedure is repeated until the extraction which has allowed a larger diversity of techniques. The extrac-
is finished [5]. tion vessel is open, so it always works under normal pressure;
As a result, Soxhlet extraction is a continuous–discrete method. microwave irradiation is focused on the sample compartment;
The assembly actually operated as a batch system since the extrac- the extraction step is completely or partially performed as in
tant acts sequentially; yet, because the extractant is recirculated the conventional Soxhlet technique (i.e., with permanent sam-
through the sample, the system also runs in a continuous manner. ple–fresh extractant contact); and no subsequent filtration is
Soxhlet Extraction can be improved in a number of ways, as Con- required [8].
ventional Soxhlet extraction which provides a number of appealing In this work, the author used as Soxhlet extraction method to
features. As a result, the sample is repeatedly brought into touch extract the geranium oil. First, collection of geranium leaves and
with fresh parts of extractant, allowing the transfer equilibrium washed with distilled water followed by drying. The soxhlet
to be displaced. High-pressure Soxhlet extraction in which the extraction method is carrying out with several organic solvents
extractor is placed in a cylindrical stainless-steel autoclave or uti- such as n-Hexane, Toluene, Methanol, Chloroform, and Water.
lise commercial or laboratory-made supercritical fluid-Soxhlet Fourier Transform Infrared Spectroscopy (FT-IR) and Gas Chro-
extractors to achieve high-pressure Soxhlet extraction. The extrac- matography analyses were used to characterise the extracted gera-
tants do not reach supercritical temperatures when using high- nium oil. Finally, author examines the Mass and Energy balances
pressure Soxhlet extraction. Automated Soxhlet extraction uses a and comparison of both soxhlet and steam distillation.

2
Y. Rajesh, N.M. Khan, A. Raziq Shaikh et al. Materials Today: Proceedings xxx (xxxx) xxx

2. Materials and methodology path, and into the empty area in the chamber housing, where the
thimble is inserted. The condenser ensures that any solvent vapour
2.1. Materials cools and drips back into the solid material chamber housing.
Warm solvent slowly fills the chamber (space in the Soxhlet appa-
The Materials required for this work are: Geranium leaves (Col- ratus) containing solid particles. The required chemicals dissolve in
lected from Mr. Labde’s Geranium Farm, Nasik), n-Hexane (Sahya- a warm solvent. When the Soxhlet chamber is filled, the syphon
dri Chemicals, Sangli), Toluene (Sahyadri Chemicals, Sangli), tube empties the chamber. The solvent was sent to the distillation
Methanol (Sahyadri Chemicals, Sangli), Chloroform (Sahyadri flask. Thimble guarantees that no solid material is transported to
Chemicals, Sangli). All the glassware (Soxhlet, Condenser, Round the still pot when the solvent moves. For maximum efficiency,
bottom flask and funnel) are used in BOROSIL grade. Distilled water cycles are repeated for several hours or days. Non-volatile com-
and Tap water used in analysis and condenser. All chemicals used pounds dissolved in the solvent during each cycle. The unit is
in analytical grade. allowed to cool after the requisite cycles are completed, and then
desirable components are separated by concentrating in a distilla-
2.2. Methodology tion still. The advantage of this method is that instead of utilising
new solvent with each cycle, the same solvent is passed through
In this work, only geranium leaves are utilised for oil extraction, the sample once and then recycled. A rotary evaporator is used
and the shrubs are collected and rinsed with tap water to remove to remove the solvent after extraction, and the extracted chemicals
any contaminants. These leaves are chopped and packed in thimble are sorted. The insoluble portion of the extracted solid stays in the
filter paper before being placed in the Soxhlet equipment for thimble, i.e., it is in material, and it is typically rejected. For extrac-
extraction. tion, 50 g of leaves and 300 ml of solvent are employed. Each time
The three major elements of a Soxhlet extractor are a percolator the experiment is carried out; different solvents are employed for
(boiler and reflux) that circulates the solvent, a thimble (typically 50 g of leaves. The following solvents are used in Soxhlet extrac-
constructed of thick filter paper) that holds the solid to be tion: n-Hexane (Boiling Point: 69 °C), Toluene (Boiling Point:
extracted, and a syphon mechanism that periodically empties the 110.6 °C), Water (Boiling Point: 100 °C), Chloroform (Boiling Point:
extractor. 61.35 °C), Methanol (Boiling Point: 61.35 °C) (Boiling Point:
The thimble is filled with the source material containing the 64.7 °C).
component to be extracted. The thimble is inserted into the Soxhlet
extractor’s main chamber. A distillation flask is used to hold the 2.3. Mass and energy Balance of Soxhlet extraction:
extraction solvent. The heating element is placed on top of the
flask. On top of the flask, the Soxhlet extractor is placed. At the The present work also carried out the mass and energy balances
top of the extractor is a reflux condenser. of each solvents n-Hexane, Toluene, Water, Chloroform, and
Fig. 2 depicts the Soxhlet apparatus. Finally, the solvent is Methanol), Geranium leaves, water resources and energy resources
heated and refluxed. The solvent is heated and vaporised, and then are used in the Soxhlet extraction of geranium oil. The Mass and
it flows through the distillation arm, also known as the vapour energy balances are detailed explanation in section 3.3.

Fig. 2. Soxhlet Apparatus.

3
Y. Rajesh, N.M. Khan, A. Raziq Shaikh et al. Materials Today: Proceedings xxx (xxxx) xxx

3. Result and discussion Fig. 4 shows the GC chromatograph of Geranium oil by compar-
ing the peak retention periods to those of reference compounds
Soxhlet extraction of geranium oil with various solvents yields performed under identical conditions, essential oil components
0.08 percent and 0.10 percent yields using Toluene and n- were identified and shown in Table 1, these are well matched with
Hexane, respectively. Gas chromatography (GC) and Fourier Trans- literature [9] of Amelia Peterson et al. and the area under the curve
fer Infrared Spectroscopy were used to characterise the Geranium shows that the principal components of essential oils are p-
Oil obtained (FTIR). Menthan-3-ol (13.31 percent), citronellol (27.41 percent), and
geraniol (43.58 percent), which would be good agreement with
the literature [10,13,16,18].
3.1. Fourier transfer Infrared Spectroscopy (FTIR):

3.3. Mass and energy balances of Soxhlet Extraction:

The chemical bonds of a molecule are detected in the form of
infrared absorption spectra by Fourier Transform Infrared Spec-
3.3.1. n-Hexane
troscopy (FTIR). The spectra provide a sample profile, or a unique
The Soxhlet extraction experiment was carried out in a batch
molecular fingerprint, which is used to screen and scan samples
process within an extractor at a temperature of 65–70 °C and
for different components. For detecting functional groups and dis-
atmospheric pressure for 2 h, with 300 ml of n-Hexane and 50 g
playing covalent bonding data, FTIR is an excellent analytical tool.
of geranium leaves. The process is done three times, resulting in
The infrared spectrum of absorption or emission of a solid liquid or
three batches with the identical solvent and conditions. Oil is
gas is acquired using FTIR. The following is the FTIR analysis of a
extracted from extract using a separating funnel after extraction
geranium oil sample Fig. 3: The investigation using Fourier Trans-
[11,12].
form Infrared Spectroscopy (FTIR) does not yield adequate results;
The oil obtained after separation is 0.15 ml and contains waxes
therefore, we switch to Gas Chromatography (GC).
from leaves for a total material mass of 150 g from three batches.
As a result, the oil yield obtained is 0.1 percent.
3.2. Gas Chromatography (GC) The energy required to heat hexane from 27 °C to 69 °C is deter-
mined using.
Gas chromatography (GC) is a method for separating compo-
Q ¼ m
C p
DT ¼ ðqVÞ
C p
DT
nents that are evaporated by heat, such as gases, liquids, and solids.
It isolates the chemical components of a sample mixture and then Where,
identifies them to determine if they are present or not, as well as Solvent Volume (V) = 300 ml = 300
10-6 m3.
their amount. The sample contains the various chemicals with Heat required to evaporate solvent (Q).
the solvent, which is subsequently heated and evaporated from Density (q) = 655 Kg/m3.
the sample injection device. With a GC system, the mobile phase Specific Heat (Cp) = 1.654 KJ/Kg K.
runs in a straight line from the sample injection unit to the column, Temperature difference (DT) = (342.15–300.15) = 42 K.
referred to as carrier gas, and then to the detector. Components Therefore, Q = 300
10-6
655
1.654
42.
were vaporised in the sample injection device and carried to the Q = 13.65 KJ = 13.65 KW-s = 13.65/3600 KW-Hr.
column by the carrier gas. The chemical mixture is split into indi- Q = 0.003792 KW-Hr.
vidual components, and the amount of each component is mea- Since 150 g of geranium yields 0.15 ml of oil hence to produce
sured using a detector. 1L of oil 1000 Kg of Geranium is required.

Fig. 3. Fourier Transform Infrared Spectroscopy (FTIR) Analysis of Geranium.

4
Y. Rajesh, N.M. Khan, A. Raziq Shaikh et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 4. Gas Chromatography (GC) Analysis of Geranium Oil.

Table 1
GC–MS data of Geranium oil.

Peak Ret. Time Component Groups % component

1 3.452 a-Pinene Terpene hydrocarbon 0.148
2 8.671 Linalool Terpenol 0.436
3 8.965 Rose oxide Oxide 0.063
4 11.471 Menthone Terpene hydrocarbon 0.091
5 12.08 p-Menthan-3-ol Terpenol 13.311
6 14.364 Citronellol Citronellol 27.411
7 17.278 Geraniol Geraniol 43.584
8 19.324 Nerol Terpenol 8.781
9 26.003 Caryophyllene Terpene hydrocarbon 0.124
10 32.550 Citronellyl propionate Citronellyl ester 0.789

For a batch 50 g geranium and 300 ml n-hexane is used hence a solvent in Soxhlet extraction [14,15]. The geranium leaf is
for 1000 Kg of geranium 6 m3 n-Hexane will be required. washed with hexane and then separated from the hexane by evap-
The energy required to heat 6 m3 n-Hexane is. oration and distillation or by utilising a separating funnel using the
Q = 6
655
1.654
42. n- hexane technique. Because of its simple oil recovery, narrow
Q = 273009.24 KJ = 13.65 KW-s = 273009.24/3600 KW-Hr. boiling point (64–69), and excellent solubilizing capacity, hexane
Q = 75.8359 KW-Hr. has been frequently employed for oil extraction [17].
Mass Balance for n- Hexane is given by. Hexane is the chemical of choice for oil extraction. Seeds or
(n-Hexane present before Extraction) = (n-Hexane present in other oil-containing fruits are crushed up and shaped into a circle
Extract Phase) + (n-Hexane accumulated in the raffinate phase). for oil extraction, which is then carried out with solvents. Allow the
Mass Balance for oil is given by. mixture to settle, and the solvent will evaporate, leaving the
(Oil initially present in Geranium) = (oil extract by n-Hexane) + extracted oil behind. Chemical extraction can be done in a variety
(Oil present in Geranium). of ways, some of which require heat and steam.
ml of n-Hexane required per gram of geranium is given by ratio
300/50 = 6 ml/g. 3.3.2. Toluene
Hence the solvent to material ratio is 6 (V/W). In a batch method, 300 ml of Toluene and 50 g of Geranium
Because of its non-polar nature, low latent heat of vaporisation leaves are used to test Soxhlet extraction at temperature (110–
(330 KJ/kg), and good selectivity of solvent, n- hexane is utilised as 115 °C) and atmospheric pressure [19,20]. Three batches are run
5
Y. Rajesh, N.M. Khan, A. Raziq Shaikh et al. Materials Today: Proceedings xxx (xxxx) xxx

with a total of two hours of experimentation time. Based on the vapour condenses and drips onto material during Soxhlet extrac-
density difference of oil and Toluene, the oil is separated from tion, losing energy in the process. As a result, it is unable to extract
the separating funnel after extraction. Because oil has a higher den- oil from geranium leaves or to extract on a big scale using Soxhlet
sity than toluene, it can be seen at the bottom of the separating apparatus, both of which are unpredictable.
funnel. Water becomes a universal solvent due to its polarity, as it dis-
The oil obtained after separation is 0.12 ml and which contains solves more compounds than any other chemical. Water molecules
waxes of leaves in it for the quantity of material 150 g from 3 have a tiny positive electric charge, whereas oxygen molecules
batches. Hence the yield of oil obtain is 0.8 %. have a slight negative electric charge, which aids in the dissocia-
The energy required to heat the toluene from 27 °C to 110.6 °C tion of ionic compounds [24].
is calculated by using.
3.3.4. Chloroform
Q ¼ m
C p
DT ¼ ðqVÞ
C p
DT
In a batch method, 300 ml of Chloroform and 50 g of Geranium
Where V = 300 ml = 300
10-6 m3. leaves are used to test Soxhlet extraction at temperature (110–
(q) = 867 Kg/m3. 115 °C) and atmospheric pressure. Three batches are run with a
Cp = 1.70 KJ/Kg K. total of four hours of experimentation time.
DT = (383.75–300.15) = 83.6 K. Chloroform produces no oil as well. Because the density of oil is
Therefore, Q = 300
10-6
867
1.70
83.6. smaller than that of chloroform, the extract obtained is a white
Q = 36.965 KJ = 36.965 KW-s = 36.965/3600 KW-Hr. homogenous mixture of chloroform in which no oil is visible and
Q = 0.010268 KW-Hr. may be separated from the top of chloroform. The energy neces-
Since 150 g of geranium yields 0.12 ml of oil hence to produce sary to evaporate the solvent is indicated below, and it can also
1L of oil 1250 Kg of Geranium is required. be used to extract oil from other materials.
For a batch of 50 g geranium and 300 ml n-hexane is used hence The energy required to heat chloroform from 27 °C to 61 °C is
for 1250 Kg of geranium 7.5 m3 Toluene will be required. determined using.
The energy required to heat 7.5 m3 Toluene is.
Q ¼ m
C p
DT ¼ ðqVÞ
C p
DT
Q = 7.5
867
1.70
83.6.
Q = 924135.3 KJ = 924135.3 KW-s = 924135.3 /3600 KW-Hr. Where V = 300 ml = 300
10-6 m3.
Q = 256.7042KW-Hr. (q) = 1490 Kg/m3.
Mass Balance for Toluene is given by. Cp = 0.98 KJ/Kg K.
(Toluene present before Extraction) = (Toluene present in DT = (334.5–300.15) = 34.35 K.
Extract Phase) + (Toluene accumulated in the raffinate phase). Therefore, Q = 300
10-6
1490
0.98
34.35.
Mass Balance for oil is given by. Q = 15.0474 KJ = 15.0474 KW-s.
(Oil initially present in Geranium) = (oil extract by Toluene) + Q = 15.0474/3600 KW-Hr.
(Oil present in Geranium). Q = 0.0041798 KW-Hr.
ml of Toluene required per gram of geranium is given by ratio Chlorinated solvents, such as chloroform, are denser than water.
300/50 = 6 ml/g. It’s the best solvent for small-scale extractions involving a little
Hence the solvent to material ratio is 6 (V/W). amount of alcohol. Because it is miscible with oils, ether, benzene,
Toluene is a non-polar solvent that is a good choice for Soxhlet CCl4, alcohol, and other solvents, chloroform is an excellent extrac-
extraction of geranium oil, but it is poisonous and must be handled tion solvent. It can be used to extract various oils from various
with care [21]. Toluene is a great solvent since it dissolves other materials, but it cannot be used to extract geranium oil [25].
organic compounds and some substances. Toluene is a chemical
that is commonly used in laboratories. 3.3.5. Methanol
In a batch method, 300 ml of Methanol and 50 g of Geranium
3.3.3. Water leaves are used to test Soxhlet extraction at temperature (62–
In a batch method, 300 ml of water and 50 g of Geranium leaves 67 °C) and atmospheric pressure. Three batches are run with a total
are used to test Soxhlet extraction at temperature (100–105 °C) of two hours of experimentation time.
and atmospheric pressure. Three batches are run with a total of Methanol does not produce any oil. The extract obtained is a
four hours of experimentation time. brown homogeneous mixture of methanol with a green precipitate
When utilising water as a solvent in Soxhlet extraction, no oil is at the bottom that extracted the entire colour of geranium leaves
obtained. Because oil has a lower density than water, it should be and may or may not contain oil, requiring further separations
removed from the top of the water, resulting in a brown uniform [25]. It is still not possible to extract oil because oil is already pre-
extract mixture. As a result, the water is unsuitable for Soxhlet sent in such small amounts that it is impossible to say whether
extraction of geranium oil [22,23]. The energy required to evapo- that precipitate contains oil or not. Even a methanol energy bal-
rate water for extraction is shown below. ance is presented below, which is useful for soxhlet extraction of
The energy required to heat water from 27 °C to 100 °C is deter- various materials.
mined using. The energy required to heat methanol from 27°Celsius to 64.7°-
Celsius is estimated using.
Q ¼ m
C p
DT ¼ ðqVÞ
C p
DT
Q ¼ m
C p
DT ¼ ðqVÞ
C p
DT
Where V = 300 ml = 300
10-6 m3.
(q) = 1000 Kg/m3. Where V = 300 ml = 300
10-6 m3.
Cp = 4.182 KJ/Kg K. (q) = 792 Kg/m3.
DT = (373.15 – 300.15) = 73 K. Cp = 2.53 KJ/Kg K.
Therefore, Q = 300
10-6
1000
4.182
73. DT = (337.85–300.15) = 37.7 K.
Q = 91.5858 KJ = 91.5858 KW-s = 91.5858/3600 KW-Hr. Therefore, Q = 300
10-6
792
2.53
37.7.
Q = 0.0254 KW-Hr. Q = 22.6625KJ = 22.6625 KW-s.
The extraction of geranium oil is frequently done with water, Q = 22.6625/3600 KW-Hr.
but the steam distillation procedure is done with steam. Water Q = 0.006295 KW-Hr.
6
Y. Rajesh, N.M. Khan, A. Raziq Shaikh et al. Materials Today: Proceedings xxx (xxxx) xxx

Table 2 Soxhlet extraction has a higher energy balance and mass balance
Comparison with Steam Distillation. than Steam Distillation. Although the yield is lower than steam dis-
Operating Parameter Steam Distillation Soxhlet Extraction tillation, this research will be useful for laboratory-scale extraction
Yield 0.15–0.2 % 0.08–0.1 % of geranium oil and other essential oils at a cheaper cost.
Operating Temperature 100–115 °C 65–70 °C
Energy Required 42.4 KW-Hr 75.83 KW-Hr
Solvent to Material Ratio 0.5 (V/W) 6 (V/W) CRediT authorship contribution statement

Yennam Rajesh: Conceptualization, Supervision, Visualization.

Methanol is an excellent solvent for extracting most chemicals; Nabeel M. Khan: Methodology. Abdul Raziq Shaikh: Methodol-
however, it is not as polar as water. It is miscible in water and has a ogy. Venkat S. Mane: Investigation, Validation. Gaurav Daware: .
high extraction yield due to its strong polarity. Although methanol Ganesh Dabhade: .
does not produce the same results with geranium oil extraction, it
does remove all miscible components and produces a green precip- Data availability
itate [26].
No data was used for the research described in the article.
4. Comparison with steam distillation
Declaration of Competing Interest
Plants are extracting geranium oil through a steam distillation
technique [25]. 1 tonne of geranium plants are placed in the distil- The authors declare that they have no known competing finan-
lation vessel, which has a steam sparger setup at the bottom. cial interests or personal relationships that could have appeared
Water is heated and evaporated by burning wood, then sparged to influence the work reported in this paper.
from the bottom of the tank at 100–115 °C for 4–6 h. Steam is
passed through the Geranium plant to extract the oil, which is then Acknowledgement
condensed using a condenser. A separator is used to remove gera-
nium oil from a water–oil combination [27–29]. Because oil and The authors are thankful to the Management and Dr. K. N. Nan-
water do not mix, the oil floats on top of the water because it durkar, Principal of K.K. Wagh Institute of Engineering Education
has a lower density than water. The oil is then syphoned off and and Research, Nashik (Affiliated to Savitribai Phule Pune Univer-
kept in a vessel. sity) for providing the laboratory and infrastructural facilities and
Geranium oil yields between 0.15 and 0.2 % after steam distilla- support.
tion. The greatest yield obtained from Soxhlet extraction using n- Also the authors are thankful to the management of ACES team
Hexane is 0.1 %. and special thanks to Dr. Sankar Chakma, Assistant Professor,
Steam distillation yields 1.5 to 2 L of oil from 1000 kg of gera- IISER Bhopal for his support and providing us the opportunity to
nium, while Soxhlet extraction with n-Hexane yields 1 L. publish our research work in scientific community.
Steam distillation has a solvent to material ratio of 0.5 (V/W),
while Soxhlet extraction has a ratio of 6 (V/W).
References
The following is the energy required in the steam distillation
process to heat and evaporates 500 kg of water: [1] B. Ali, Naser Ali Al-Wabel, Saiba Shams, Aftab Ahamad, Shah Alam Khan, Firoz
Anwar, Essential oils used in aromatherapy: A systemic review, Asian Pacific
Q ¼ m
C p
DT ¼ ðqVÞ
C p
DT Journal of Tropical Biomedicine 5 (8) (2015) 601–611.
[2] C.-M. Lo, J. Han, E.S.W. Wong, Chemistry in Aromatherapy – Extraction and
m = 500 Kg. Analysis of Essential Oils from Plants of Chamomilla recutita, Cymbopogon
Cp = 4.182 KJ/Kg.K. nardus, Jasminum officinale and Pelargonium graveolens, Biomedical &
Pharmacology Journal 13 (3) (2020) 1339–1350.
DT = (373.15–300.15) = 73 K. [3] L.K. Narnoliya, J.S. Jadaun, S.P. Singh, The Phytochemical Composition,
Therefore Q = 500
4.182
73. Biological Effects and Biotechnological Approaches to the Production of High
Q = 152643KJ = 152643 KW-s = 152643/3600 KW-Hr. Value Essential Oil from Geranium, Essential Oil Research (2019) 327–352.
[4] P.B. Gomes, V.G. Mata, Aĺırio E, Rodrigues, Production of rose geranium oil
Q = 42.4 KW-Hr.
using supercritical fluid extraction, Journal of Supercritical Fluids 41 (2007)
The energy required to heat the water in steam distillation is 50–60.
about 42.4 KW-Hr and energy required to heat the n-Hexane is [5] B. Tesfaye, T. Tefera, Extraction of Essential Oil from Neem Seed by Using
about 75.83 KW-Hr for 1 ton of material [30]. The summary of Soxhlet Extraction Methods, IJAEMS 3 (6) (2017) 646–650.
[6] M.D. Luque de Castro, L.E. GarcõÂa-Ayuso, Soxhlet extraction of solid
comparison details are listed in Table 2. materials: an outdated technique with a promising innovative future, Anal.
Chim. Acta 369 (1998) 1–10.
[7] M.D. Luque de Castro, F. Priego-Capote, Soxhlet extraction: Past and present
5. Conclusion panacea, J. Chromatogr. A 1217 (2010) 2383–2389.
[8] P.u. Wang, Q. Zhang, Y. Wang, T. Wang, X. Li, L. Ding, G. Jiang, Evaluation of
Soxhlet extraction, accelerated solvent extraction and microwave-assisted
This work concludes that employing the Soxhlet extraction extraction for the determination of polychlorinated biphenyls and
method to extract geranium oil is a promising way for extracting polybrominated diphenyl ethers in soil and fish samples, Anal. Chim. Acta
oil using organic solvents (n-Hexane, Toluene, Chloroform, Water, 663 (2010) 43–48.
[9] A. Peterson, S. Machmudah, Bhupesh C Roy, Motonobu Goto, Mitsuru Sasaki
Methanol). Soxhlet extraction yields of 0.1 percent and 0.08 per- and Tsutomu Hirose, Extraction of essential oil from geranium (Pelargonium
cent with n-Hexane and Toluene solvents, respectively. The graveolens) with supercritical carbon dioxide, Journal Chemical Technology,
obtained oil sample was first examined using Fourier Transform Biotechnology 81 (2006) 167–172.
[10] B. Tesfaye, T. Tefera, O. Misikir, G. Tsegaye, Extraction and comparison of
Infrared Spectroscopy (FTIR), but the results were unsatisfactory.
essential oil from neem seed by using soxhlet extraction and simple
We subsequently examined the oil using Gas Chromatography distillation methods, International Journal of Engineering Technologies and
(GC). The components of Geranium oil can be determined using Management Research 5 (9) (2018) 74–81.
gas chromatography (GC), it was noticed that p-Menthan-3-ol [11] H. Rodolfo Juliani, A. Koroch, J.E. Simon, N. Hitimana, A. Daka, Lalasoa
Ranarivelo & Petrus Langenhoven, Quality of Geranium Oils (Pelargonium
(13.31 %), citronellol (27.41 %) and Geraniol (43.58 %) has major Species): Case Studies in Southern and Eastern Africa, J. Essent. Oil Res. 18
proportion in essential oil which is good agreement literature. (2006) 116–121.

7
Y. Rajesh, N.M. Khan, A. Raziq Shaikh et al. Materials Today: Proceedings xxx (xxxx) xxx

[12] Mohamed Nadjib Boukhatem, Abdelkrim Kameli, Mohamed Amine Ferhat, [22] B. Pavlic, S. Vidovic, J. Vladic, R. Radosavljevic, Zoran Zekovic, Isolation of
Fairouz Saidi and Maamar Mekarnia, Rose geranium essential oil as a source of coriander (Coriandrum sativum L.) essential oil by green extractions
new and safe anti-inflammatory drugs, Libyan, J. Med. 8 (2013) 22520. versus traditional techniques, The Journal of Supercritical Fluids 99 (2015)
[13] F.S. Sharopov, H. Zhang, W.N. Setzer, Composition of geranium (Pelargonium 23–28.
graveolens) essential oil from Tajikistan, American Journal of Essential Oils and [23] A.Z. Kakasy, É. Lemberkovics, B. Simándi, L. Lelik, É. Héthelyi, I. Antal, É. Szöke,
Natural Products (AJEONP) 2 (2) (2014) 13–16. Comparative study of traditional essential oil and supercritical fluid extracts of
[14] Neetu Jain, K. K. Aggarwal, K. V. Syamasundar, S. K. Srivastava and Sushil Moldavian dragonhead, Dracocephalum moldavica L, Flavour and Fragrance
Kumar, Essential oil composition of geranium (Pelargonium sp.) from the Journal 21 (2006) 598–603.
plains of Northern India, Flavour and Fragrance Journal, 16 (2001) 44-46. [24] Z. Mustafa, Ozel, Hilal Kaymaz, Superheated water extraction, steam
[15] B.R. Rajeswara Rao, P.N. Kaul, K.V. Syamasundar, S. Ramesh, Water soluble distillation and Soxhlet extraction of essential oils of Origanum onites, Anal
fractions of rose-scented geranium (Pelargonium species) essential oil, Bioanal Chem 379 (2004) 1127–1133.
Bioresour. Technol. 84 (2002) 243–246. [25] G. Wenqiang, L.i. Shufen, Y. Ruixiang, T. Shaokun, Q. Can, Comparison of
[16] M. Boukhris, M.S.J. Simmonds, Sami Sayadi and Mohamed Bouaziz, Chemical essential oils of clove buds extracted with supercritical carbon dioxide and
composition and biological activities of polar extracts and essential oil of rose- other three traditional extraction methods, Food Chem. 101 (2007) 1558–
scented geranium, Pelargonium graveolens, Phytother. Res. (2012) 1–8. 1564.
[17] P.B. Gomes, V.G. Mata, A.E. Rodrigues, Characterization of Portuguese-Grown [26] Y.C. Wong, M.Y. Ahmad-Mudzaqqir, W.A. Wan-Nu, Extraction of Essential Oil
Geranium Oil (Pelargonium sp.), J. Essent. Oil Res. 16 (2004) 490–495. from Cinnamon (Cinnamomum zeylanicum), Orient. J. Chem. 30 (1) (2014)
[18] M. Jalali-Heravi, BehroozZekavat, Hassan Sereshti, Characterization of 37–47.
essential oil components of Iranian geranium oil using gas chromatography– [27] S. Vahid Mortazavi, Mohammad H. khaje b, Habib Mirzaei, Mahdi Jafari,
mass spectrometry combined with chemometric resolution techniques, J. Fereshteh Golmohammad, Extraction of essential oils from Bunium persicum
Chromatogr. A 1114 (2006) 154–163. Boiss. using superheated water, Food and Bioproducts Processing, 8 (2010)
[19] Pandey Pragya, Upadhyay R.K., Singh V.R., Padalia R.C., Kumar Rakesh, 222–226.
Venkatesha K.T., Tiwari A.K., Singh Sonveer and Tewari S.K., Pelargonium [28] M. Khajenoori1, A. Haghighi Asl, F. Hormozi , M.H. Eikani And H. Noori Bidgoli,
graveolens L. (Rosescented geranium): New hope for doubling Indian farmers’ Subcritical Water Extraction Of Essential Oils From Zataria Multiflora Boiss,
income, Environment Conservation Journal, 21 (1&2) (2020) 141-146. Journal of Food Process Engineering, 32 (2009) 804–816.
[20] A.S. Shawl, T. Kumar, N. Chishti, S. Shabir, Cultivation of Rose Scented [29] Mohammad H. Eikani, Fereshteh Golmohamma , Soosan Rowshanzamir,
Geranium (Pelargonium sp.) as a Cash Crop in Kashmir Valley, Asian Journal of Subcritical water extraction of essential oils from coriander seeds
Plant Sciences 5 (4) (2006) 673–675. (Coriandrum sativum L.), Journal of Food Engineering, 80 (2007) 735–740.
[21] K.G.D. Babu, V.K. Kaul, Variation in essential oil composition of rose-scented [30] M. Virot, V. Tomao, G. Colnagui, F. Visinoni, F. Chemat, New microwave-
geranium (Pelargonium sp.) distilled by different distillation techniques, integrated Soxhlet extraction An advantageous tool for the extraction of lipids
Flavour and Fragrance Journal 20 (2005) 222–231. from food products, J. Chromatogr. A 1174 (2007) 138–144.

View publication stats