Effect Of Long Time Distillation To Yields and Compotitions of Kaffir Lime Leaves Oil

Using Steam Distillation

Risna Silvianti*, Rhezaldian Eka Dharmawan*, Vivi Nurhadianty dan Chandrawati Cahyani
Department of Chemical Engineering , Brawijaya University , Malang, 65145
Essential Oil Institute University of Brawijaya

ABSTRACT
Distillation of kaffir lime leaves with water content of 15 2% using distillation method steam
is carried out for 4 hours, 6 hours and 8 hours. Variations of distillation give significant effect
on yield and composition of kaffir lime leaves oil composition . The longer distillation yield is
increased. The yield of oil produced at the distillation time is 4 hours, 6 hours and 8 hours
respectively by 0.98%, 1.27% and 1.33%. Number of identified compounds
produced tends to increase and the distillation time of 6 hours is long optimal distillation with
linalool content (2.62%), citronellal (85.83%), citronelol (3.01%) and -citronellyl acetate
(3.09%).

INTRODUCTION
At the distillation of essential oil , long distillation needs to be considered because the oil glands
are in the vacoula in a plant tissue that categorized as metabolite results secondary and
responsible against a distinctive aroma (Guenther, 1987).The distillation process takes time the
old one having to open oil glands to obtain essential oil (Guenther, 1987).
Kaffir lime leaves oil composed over terpenoid hydrocarbon complexes,terpenoids oxygenated
and sesquiterpen
which is utilized in the flavor industry,pharmacy, and food (Sawamura, 2010). Koswara (2009)
mentions that
kaffir lime leaves oil contain sitronelal (81.49%), citronelol (8.22%), linalool (3.69%), geraniol
(0.31%) and components others (6.29%).
Hidayat (1999)using the water distillation method for 8 hours with kaffir lime leaf sample
from Ponorogo and Madiun produces citronellal as much as 84.202%. While Srisukh et al.
(2012) using kaffir lime leave comes from Thailand and China by steam distillation method for
4 hours produces sitronelal as much as 80.04%. According to Sawamura (2010), the old
distillation can be causing changes in composition essential oil compounds produced.
The purpose of this research is to to know the effect of the old distillation kaffir lime leaves
from Blitar with a steam distillation method to the yield and composition of kaffir lime leave
oil.

MATERIALS AND METHODS

Tools and materials

Main equipment in this research is a pilot scale steam distillation unit. Analytical tools include
erlenmeyer,
moisture balance, separation funnel, balance sheet analytic, pycnometer, pipette, glass bottle,
vacuum filtration, syringe and tools instrumentation GC-MS (Gas Chromatography - Mass
Spectrometry) brand Shimadzu type QP2010 Plus. The material used is Na2SO4 anhydrous
(technical grade) and kaffir lime leaves from the Nursery Institute Atsiri Universitas Brawijaya
in the Village Kesamben, Blitar.

Method

This research is using steam distillation method. Processing and analysis data in the
determination of best treatment from distillation of kaffir lime leaves using qualitative
descriptive analysis and quantitative. Data that used obtained from the instrumentation test
results GC-MS and its distillation results including density and yield of kaffir lime leaves oil.

The study design uses variation of the distillation time for 4 hours, 6 hours and 8 hours. Steps
research as follows:
1. Pretreatment of lime leaves.
2. Drying kaffir lime leaves with dry air method to moisture content reaching 15 2%.
3. Distillation of kaffir lime leaves with using kaffir lime leaves raw materials as much as 2.5
kg.
4. Separation of distillate (oil layer kaffir lime leaves and water layer) using separating funnel
and
addition of anhydrous Na2SO4 to get kaffir lime oil which is free of water content.
5. Oil leaves of kaffir lime obtained then calculated mass value type, yield and analyzed
composition of chemical compounds with using the GC-MS tool.
RESULTS AND DISCUSSION

The Effect of Long Time Distillation to the yield of Kaffir Lime Leave Oil

The yield of leaf lime oil yield from the distillation time of 4 hours, 6 hours and 8 hour shown
in Figure 1.
From Figure 1. the yield of kaffir lime leaf oil increase with the longer distillation. The yield
that obtained from this research ranged between 0.98 - 1.33% and kaffir lime leaves oil with
good quality has a yields ranging from 1 - 1.5% (Herb, 2008). So that it can inferred leaf lime
oil the resulting quality is sufficient both in accordance with the literature.
Yield (%)

Time Of Distillation (hr)

Figure 1. Effect of Long Time Distillation to Yields of Kaffir Lime Leaves Oil

The lowest oil yield obtained at 4 hours distillation time ie by 0.98% due to the amount of
steam heat that is in contact with the material still very little, so the diffusion process oil from
oil glands to the material surface is also still relatively small. At the distillation time 4 hours
consists of components of molecular weight oil small, while the oil component with a large
molecular weight yet evaporated.
At the distillation time is 6 hours oil yield is obtained as big as 1.27%. Increased distillation
time causing the amount of hot steam that is contact with more and more materials, so the
process of oil diffusion increasingly
increased. In addition, the oil component with a large molecular weight starting evaporated so
that the yield is increased.
At the distillation time is 8 hours obtained oil yield of 1.33% this is due to the resulting steam
more and more, so that the steam is hot the contact with the material increases. This condition
causes the diffusion process
increased oil and components oil with molecular weight the greater has been evaporated, so
the yields progressively great (Tekper Sentosa, 2004). According to Rusli (1979), the longer
distillation then the more heat received by materials and processes increased oil diffusion. Oil
that diffuses to the surface of the material easily carried away with steam and extracted because
of its essential oil properties volatile (flying oil).
The increase of leaf oil yield orange kaffir on 6 hours long distillation quite significant that is
equal to 29.60%
against a 4 hour refinery. While at the distillation time of 8 hours percentage increase of
rendement of citrus leaves oil kurut only amounted to 4.72% against distillation 6 hours. If
process distillation continued over 8 hours, then it is feared can cause color and aroma of citrus
leaves oil the resulting kurut is not good due to thermal decomposition of the material lime
leaves (Yusoff, et al., 2013).

The Effect of Long Time Distillation to the Composition of Kaffir Lime Leave Oil
Distillation of kaffir lime leaves with steam distillation method is carried out for 4 hours, 6
hours and 8 hours. Variation long distillation gives effect significant to the composition of the
kaffir lime leaves oil .
Kaffir lime leaves oil obtained from each treatment in compound type and composition analysis
active contained using Gas Chromatography - Mass Spectometry (GC-MS), so the resulting
data of chromatogram as follows:

Figure 2. Chromatogram of Kaffir Lime Leaves Oil at time distillations 4 hour

Figure 3. Chromatogram of Kaffir Lime Leaves Oil at time distillations 6 hour

Figure 4. Chromatogram of Kaffir Lime Leaves Oil at time distillations 8 hour

On the indicated chromatogram by Figures 2, 3 and 4, can be seen that the composition of the
compound is identified most produced on kaffir lime leaves oil with long time ditillation of 6
hours shown with the peak number of areas that appear in Figure 3.
On the 4 hour distillation producing 12 unidentified compounds,on a 6 hour refinery produces
17 unidentified compounds and on 8 hour refinery produces 15 unidentified compounds.
Difference in number and composition compounds on each other long distillation can be caused
by the difference in the amount of steam produced.
According to David (2000) on the old process Different extractions will result different vapor
compositions. Increasingly long distillation process, will causing the steam to form and
terpenetrasi in grandular oil as well more and more, so the components oil constituents that can
carried away and extracted by steam as well more and more. In the old distillery 6 hours, the
compound produced more complex compared to old distillation 4 hours, due to the amount of
steam formed at the distillation time 6 more hours, so it can carrying that oil component diffuses
to the surface of kaffir lime leaves more. While on the old distillation 8 hours composition of
the compound the resulting decrease because of the complex reaction so there are some
compounds that lost or merged into one. Besides it, the type of component produced on long
distillation 8 hours, not far away different from the distillation time of 6 hours, so with the old
increase distillation is not produced difference composition of kaffir lime leave oil significant.

Figure 5. Effect of Long Time Distillation to Compound of Majour Component

Figure 5. shows the levels the major compound produced on lime leaves oil with long time
different distillation experiencing changes. This can caused by the occurrence of reactions
secondary during the distillation process such as complex reactions that involve interactions
between internal compounds lime leaves oil so leaf oil compounds Kaffir lime changes.
According Turek (2013), components organic compounds contained within essential oils have
properties that are not stable and thus susceptible to occurrence changes in molecular structure
of each component. Component constituents of essential oils can be with easily converted into
other compounds through oxidation reactions, polymerization,isomerization, cyclization or
dehydrogenation which can occur enzymatically and chemically. Reactions it can occur due to
heating which is too long, the presence of oxygen and high acidity level.
From the research results obtained levels citronellal ranged between 84.49 - 85.83% or higher
than levels sitronelal obtained by Koswara (2009) equal to 81,49% and Srisukh et al. (2012) of
80.04%. The citronellal levels are obtained higher than with literature caused by pretreatment
on citrus leaf material kurut ie the drying process with dry air. According to Wijaya (2010),
drying kaffir lime leaves can improve yield and composition of volatile compounds is produced
on the oil of kaffir lime leaves .

Figure 6. Effect of Long Time Distillation to Compound of Citronellal

From Figure 6. look more long distillation, compound levels sitronelal tends to increase up a
certain time limit then occurs decline but not very significant. The optimal refining duration
for producing the highest citronellal levels is for 6 hours. Increased levels citronellal at 4 hours
distillation time up to 6 hours due to the old 4 hour distillation, steam heat contact with material
not enough for make the whole sitronelal in the leaf lime juice extracted. But if it's long
distillation done over 6 hours, the resulting citronellal content decreased to 84.49%. This is due
to the old distillation 8 hours, compound level with more molecular weight bigger and boiling
point higher increased like benzoic acid, dodecanol and linalyl acetate affects the citronellal
levels generated.
Decreased levels of citronellal on long an 8 hour refinery allegedly caused by citronellal
dehydration reaction becomes hydrocarbon terpenes that occur during the distillation process
due too long heating and level high acidity. The longer distillation, pH distillate produced will
be lower, so it can accelerate complex reactions which leads to changes in the compound
constituent of oil. Major compounds such as citronellal, linalool and citronellol is a type of
monoterpen compound oxygenated most dominant in leaf lemon leaf oil is wrong one
suspected reaction causing a decrease in levels citronellal in the distillation time 8 hours is a
citronellal dehydration reaction hydrocarbon terpenes that occur during the distillation process
due the heating is too long.
From Table 1. it shows that it is long 6 hour distillation is long . Optimal distillation due
obtained rendemen of 1.27% with the content of citronellal compounds highest of 85.83%. Oil
prices lime leaves vary depending at levels of citronellal compounds. According to data from
the original essential oil company People's Republic of China, Khunsan Yalong Trading Co.,
Ltd, essential oil with 85% citronellal content worth 140.92 USD / kg. Also on the old
distillation 8 hours actually produced levels lower sitronelal is equal to 84.49% which resulted
in the selling price lower oil. At the distillation time 6 hours amount more identified compounds
compared to the distillation time 4 hours and 8 hours. The compound composition contained
in citrus leaves oil kurut become one of consideration in determining the selling price related
to oil quality lime leaves. According to Rennecius (1999) components of compounds in leaf
lemon leaf oil comes from of the terpenoid compound class can determine the intensity of odor,
aroma, and the selling value of kaffir lime oil. Distillation 6 hours produce components of most
terpen compounds, so the quality of citrus leaves oilthe resulting kurut is higher compared to
the distillation time 4 hours and 8 hours.
Table 1 . Ratio of Yields, Citronellal Compound,and Identification Compound at Each Time
Distillation
From Table 1. it shows that it is long 6 hour distillation is long.Optimal distillation due obtained
rendemen of 1.27% with the content of citronellal compounds highest of 85.83%. Oil prices
lime leaves vary depending at levels of citronellal compounds. According to data from the
original essential oil company People's Republic of China, Khunsan Yalong Trading Co., Ltd,
essential oil with 85% citronellal content worth 140.92 USD / kg. Also on the old distillation
8 hours actually produced levels lower sitronelal is equal to 84.49% which resulted in the
selling price lower oil. At the distillation time 6 hours amount more identified compounds
compared to the distillation time 4 hours and 8 hours.
The compound composition contained in citrus leaves oil kurut become one of consideration
in determining the selling price related to oil quality lime leaves. According to Rennecius
(1999) components of compounds in leaf lemon leaf oil comes from of the terpenoid compound
class can determine the intensity of odor, aroma,and the selling value of kaffir lime oil.
Distillation 6 hours produce components of most terpen compounds, so the quality of citrus
leaves oil the resulting kurut is higher compared to the distillation time 4 hours and 8 hours.

CONCLUSIONS AND RECOMMENDATIONS

The conclusions obtained from this research is:

1. The longer distillation yields the resulting increase.The resulting oil yield at the distillation
time of 4 hours, 6 hours and 8 hours in a row 0.98%, 1.27% and 1.33% respectively.
2. The longer the distillation amount the identified compounds produced tends to increase and
long distillation 6 hours is duration of optimal distillation with linalool levels
(2.62%),citronellal (85.83%), citronelol (3.01%) and -citronellyl acetate (3.09%).
Suggestions that can improve and developed this research are:
1. Need for temperature control and T control on cooling water at condenser using chiller for
improve cooling effectiveness.
2. Steam leak attempted tackled in order to increase rendement and the composition of lime
leaves oil resulting from.
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