I.

Experiment Title : Isolation of Ginger Oil

II. Experiemnt Date : February 27th, 2018 (10.30-16.30)
III. Experiment purpose :
1. Selecting the required equipment in accordance with the experiments
performed
2. Selecting materials needed in accordance with the experiments performed
3. Isolating ginger oil from the ginger rhizome in proper way
IV. Basic Theory
Ginger (Zingiber officinale Roscoe) is a plant that belongs to the
Zingiberaceae family. The plant is indigenous to warm tropical climates,
particularly southeastern Asia. It is extensively ultivated in India, China,
Africa, Jamaica, Mexico and Hawaii (Evans, 1989). Ginger products, such as
the essential oil and oleoresin, are internationally commercialized for use in
food and pharmaceutical processing. The essences due to their chemical
nature are volatile at ordinary room temperature and might be called volatile
oils, ethereal oils or essential oils. Various techniques have been employed to
extract this valuable fraction of the plant material namely by water, steam
istillation or application of microwave and liquid carbon dioxide (Sellar,
2001).
The essential oils are composed of monoterpene hydrocarbons,
sesquiterpene hydrocarbons and oxygenated monoterpene. Although the
latter has the least concentration but is the major contributor to the taste and
aroma of food substances (Parthasarathy et al., 2008).
The recovery of the essential oils of ginger depend on variety and
origin of the plant as well as the cultivation, humidity at the time of harvest,
the methods of extraction and to some extent on the age of the plant
(Onyenekwe and Hashimoto, 1999). Although ginger essential oils is yellow,
the intensity of colour, aroma and taste varies according to the originated
place of cultivation (John and Ferreira, 1997; Purseglove et al., 1981;
Guenther, 1975).The chemical composition of essential oils of ginger has
been identified and quantified by means of GC-MS or GC with flame
ionization detector applications (Sultan et al., 2005; Singh et al., 2008).
The Imperial Institute London gets 4.0% of the oil from the
distillation of water and steam, while the Vrier in northern Travancore with
 the distillation of water from the air-dried ginger powder gets 0.8% oil. The
properties of both oils can be seen in Table 1.1
The result of the research of Bogor Agricultural Product Center
(BBIHP) Bogor proved that unpeeled rhizome yields rendemen 2,4-3,6%,
while peeled only 1.9-3,0% with water content of rhizome about 10-12%. PT
Djasulawangi, Jakarta proved the distillation of fresh ginger without drying,
was ground roughly and put in a distillation boiler with local white ginger
raw material yielding 0.2% rendement, equivalent to 2% dried ginger,
although the yield was only 0.2-0.3% refining fresh ginger without drying is
still quite profitable.(Susihono, Wahyu, 2011)
According to Kepen and Djatmiko1, ginger oil can be obtained by
distillation of dry rhizomes with a yield of 1-3%. The properties of ginger oil
include volatile oils, greenish to yellowish, but are generally light yellow
which is a rather viscous, distinctive and durable odor, stable in weak alkali
but unstable in acids and concentrated bases, soluble in benzyl benzoate,
diethyl phthalate and mineral oil in all comparisons, but slightly soluble in
alcohol, but not soluble in propylene glycol.
Tabel.1 the characteristic of Ginger Oil by Imperial Institute London
and North Travancore
Value
Karakteristik Vrier at Travancore
Imperial Institute at London
Utara
Specific geavity d15 0.881 d15 0.8905
Optical wheel -43˚45’ -5˚12’
Refraction index nD201.492 nD301.4859
Acidity number 1.5 0.9
Esteric Number 2.9 6.1
Esteric number after
33.1 72.7
asetilation
Source : S. Keteren and B. Djatmiko (1978)

Extraction
 We can separate an analyte and an interferent if there is a significant
difference in at least one of their chemical or physical properties. Table 7.4
provides a partial list of separation techniques, classified by the chemical or
physical property being exploited.

Basis of Separation Separation Technique

Filtration; dialysis; size-exclusion
Size
chromatography
Mass or density centrifugation
Complex formation masking
Distillation; sublimation;
Change in physical state
recrystallization
Precipitation; electrodeposition;
Change in chemical state
votalization
Extraction
Partiloning between phase
chromatography

Continuous Extractions

A continuous extraction of a solid sample is carried out using

a Soxhlet extractor (Figure 7.24). The extracting solvent is placed in the
lower reservoir and heated to its boiling point. Solvent in the vapor phase
moves upwards through the tube on the far right side of the apparatus,
reaching the condenser where it condenses back to the liquid state. The
solvent then passes through the sample, which is held in a porous cellulose
filter thimble, collecting in the upper reservoir. When the solvent in the upper
reservoir reaches the return tube’s upper bend, the solvent and extracted
analyte are siphoned back to the lower reservoir. Over time the analyte’s
concentration in the lower reservoir increases.
 Figure 1 Soxhlet extractor. See text for details

After placing the sample and the solvent in a sealed digestion vessel, a
microwave oven is used to heat the mixture. Using a sealed digestion vessel
allows the extraction to take place at a higher temperature and pressure,
reducing the amount of time needed for a quantitative extraction. In a Soxhlet
extraction the temperature is limited by the solvent’s boiling point at
atmospheric pressure. When acetone is the solvent, for example, a Soxhlet
extraction is limited to 56oC, but a microwave extraction can reach 150oC.

Two other continuous extractions deserve mention. Volatile organic

compounds (VOCs) can be quantitatively removed from liquid samples by a
liquid–gas extraction. As shown in Figure 7.25, an inert purging gas, such as
He, is passed through the sample. The purge gas removes the VOCs, which
are swept to a primary trap where they collect on a solid absorbent. A second
trap provides a means for checking to see if the primary trap’s capacity is
exceeded. When the extraction is complete, the VOCs are removed from the
primary trap by rapidly heating the tube while flushing with He. This
technique is known as a purge-and-trap. Because the analyte’s recovery
may not be reproducible, an internal standard is necessary for quantitative
work.
 Figure 7.25 Schematic diagram of a purge-and-trap system for
extracting volatile analytes. The purge gas releases the analytes, which
subsequently collect in the primary adsorbent trap. The secondary adsorption
trap is monitored for evidence of the analyte’s breakthrough(Harvey, David,
2016)

V. Tools and Materials

a. Tools
1. Extraction equipment (soxhlet) 1 piece
2. Evaporator 1 piece
3. Funnel 1 piece
4. Mortar 1 piece
5. Refractometer 1 piece
6. Hot plate 1 piece
7. Heating mantle 1 piece
8. Graduated cylinder 1 piece
9. Another glass equipment sufficient
b. Materials
1. Sodium sulphat anhydrate sufficient
2. Dry ginger 10-3- grams
3. Petroleum eter 100 ml
VI. Lanes Work
1. Isolation of Ginger Oil
 2. Determine the mass of water

VII. Experiment Result

No. Prosedur Percobaan Hasil Pengamatan Dugaan/R
Sebelum Sesudah
 I. of Ginger Oil
1. Isolated n-heksane : n- heksane : dark In theory, index bias From this
Ginger colorless yellow of n- heksane 1,378- experiment we
- ashed 1.381 can conclude that
- easured Dry ginger : Ginger : wet, brown, And index bias of mass of ginger oil
- ried
yellowish smell ginger reduce ginger oil is 1,486- is 1,4 grams
Dry Ginger 1,492
- Delicated
Extracted : brown Rendement mass
solution and white (Source : Fatriani of ginger oil :
Ginger Powder residue vol08, 2007) 14%
- acked by filter paper with up and down bonded
- easured until 3 – 5 grams Na2SO4 anhydrous : In theory rendement
- ntered into extract soxhlet brown solution + of ginger oil is 1,9-
- ntered protelium ether solvent 1 ml into the flask extractor
- xtracted until result the colorless product 3,0%
Decantation : brown
olorless xtraction solution (Source : Balai Besar
- ait until the fluid drop to the extractor flsk Industri Hasil
- Opened the soxhlet
- ake the sample Entered into Pertanian, Tanpa
- eturned the soxhelt set as before evaporator= gingger Tahun)
- teamed the solvent in extractor flask until saturated in soxhlet tools
- ept the volume of solvent to not fall down oil :dark brown

olvent xtract
Mass : 1,4 grams
- dded a O anhidrous
2 4
- eparated by filtration The number of
dropped solvent : 11
esidue iltrate
times

- eighed - easured Rendement mass of

ginger oil : 14%
ass efractive
index
- alculated

ield of oil
 Index bias of n-
heksane = 1,362211

Index bias of ginger

oil = 1,37253j

2. Determine the mass of water Wet gingger : Wet ginger + entered The mass of water
brown colour into an oven : in ginger is 60%
Dry, yellow colour
Mass of wet
ry ginger powder
gingger : 1 gram Mass of dry ginger :
- eighed about 1 gram 0,4 gram
- ried In theory, mass of
- eighed again mass of water = water from fresh
- ritten the mass 1 grams – 0,4 grams ginger 88,17%
- epeated the heating until the content mass obtained = 0,6 grams = 60%
(Source : Fathona,
The content of Difa, 2011)
water ginger
VIII. Analysis and Explanation

About 30-50 grams of ginger powder is packed with filter paper. The top of
filter paper is bonded with rope to help take it from reflux. The reflux is packed in
the place. At the bottom rounded flask filled with n-hexane solution as the solvent in
the extraction ginger process. The choosing of n- hexane, because this is the most
soluble solvent than others. N-hexane is the highest solvent. Its smell like petroleum,
its colorless, and solute substance. Also added a boiling stone, to help the boiling
process conduct perfectly.

Heater putted at the bottom of rounded flask, to heat the n-hexane, and
evaporate. The n-hexane vapor will enter the cooler tube which has been filled with
cool water. the vapor will cool down and change become n-hexane solution, that will
drop the ginger powder. each drop of n-hexane will change the color of n-hexane at
the rounded flask, that will contain the ginger extract. the extraction process is
stopped when the n-hexane in the reflux is colorless, while the n-hexane in the
rounded flask is yellowish color. And added some spoon of Na2SO4, to help the
filtration process. Na2SO4 will bound the impurities substance from the rest of
heating process.

After the n-hexane in the rounded flask is yellow, so it will evaporate again to
make sure that the n-hexane is evaporate perfectly. So, the ginger oil result will be
pure. This may take longer time, because it done with 500C water as heater and at 50
rpm with evaporator equipment.

The result of evaporation is 1.4 grams ginger oil, with brown color and thick
texture. After the ginger oil ready, it comes to biased index test using refractometer.
Firstly, the layer of refractometer is cleaned with water and after that dried with
tissue paper and then cleaned with n-hexane solution. The reason why we use n-
hexane as secondary cleaning process is because n-hexane is the solvent of ginger
powder. After that add about 3 drops of ginger oil into refractometer to check the
biased index of ginger oil. We have to lighting the light resivior to help observing the
biased index. Because it has no mirror to focus the sun light like microscope, but it
use light to help observing biased index. The result of biased index is 14 %.
 The second experiment is measuring the percentage of water in the ginger.
Firstly, the ginger is weighed and sliced as thin as possible. It will help the heating
process, so the water from ginger will evaporate quicker. It enters into oven about 30
minutes until the ginger dry perfectly. After it dry weighed it again to calculate the
mass of water in ginger. the percentage of water is 60%.

IX. DISCUSSION
From the experiment about 1.4 grams of finger oil is obtained from extraction
process. It must be littler, because the process of evaporator is too quick so the n-
hexane cannot evaporate perfectly. It means that in ginger oil there is more n-hexane
can not evaporate perfectly. So it will influence the result of index biased
calculation, rendement calculation and experiment ginger oil result. Evaporation
process should be done at longer time, so it will evaporate the n-hexane perfectly.
X. . CONCLUSION

From the experiment we can conclude that, mass of ginger oil is 1,4 grams,
rendement mass of ginger oil is 14% and percentage of water in ginger is 60%.
XI. References

Harvey, David. 2016. Classifying Separation Techniques.

https://www.google.co.id/url?sa=t&source=web&rct=j&url=https://chem.li

bretexts.org/Textbook_Maps/Analytical_Chemistry_Textbook_Maps/Map

%253A_Analytical_Chemistry_2.0_(Harvey)/07%253A_Collecting_and_Pr

eparing_Samples/7.6%253A_Classifying_Separation_Techniques&ved=2a

hUKEwjW1aKHttXZAhWFvY8KHUAWDi8QFjAAegQIAxAB&usg=AO

vVaw34DcC4e1STuDAO1kpK4VB. Accessed on Monday, March5, 2018

at 9:30 pm.

Ketaren, S. dan B. Jatmiko. 1978. Minyak Atsiri Bersumber dari Batang dan Akar.

Departemen Teknologi Industri Hasil Pertanian. Fameta. Institut Pertanian.

Bogor.

Susihono, Wahyu. 2011. Widyariset, Vol. 14 No.3 (e-book).

https://www.google.co.id/url?sat=t&source=web&rct=j&url=http://widyaris

et.pusbindiklat.lipi.go.id/index.php/widyariset/article/viewFile/450/372&ve

d=2ahUKEwjzmeDds9XV=ZahVHa7wKHcu5BgcQFjAAegQlBxAB&usg

=AovVaw21Bb3RCPintEBY0hbqRKIK Accessed on Monday, March5,

2018 at 9:30 pm.

XII. Attachment

I. Answer and Quetions

1. Make the research question about the experiments !
- Why in experemient is used petroleum ether?
- Why in this experiment added Na2SO4 anhydrous?
- What is the colour changed in before and after?

2. Explain briefly the working principal of soxhlet extraction used in this

experiment!
The working principle of soxhlet extraction in this experiment is the process
of separating and purifying a component (extract) from a natural material
based on the difference of the boiling point using a volatile solvent (having a
large boiling point difference with the desired extract)
3. When the solvent separation using evaporator tool? Give a reason!
In the experiment of ginger oil isolation from ginger rhizome above using
soxhlet tool, but when solvent separation using evaporator tool then the
solvent used is volatile, because the working principle of evaporator that is
same with soxhlet extraction is by evaporating solvent. But the disadvantage
of the use of evaporator is that most of the essential oil content will swab
because it is volatile.
4. Based on the yield of essential oil obtained, how is the drying and smoothing
of ginger powder effect on yield? Explain!
The way of drying and smoothing of ginger powder also affects the yield of
essential oils:
In the drying process, if done by using high temperature will damage ginger
oil, due to the nature of oil that can evaporate, then to prevent it ginger
powder dried in the sun for 3 days with constantly constant heat constant. In
addition, during the extraction process, a set of tools (controlled temperature)
is used to heat the petroleum solvent with the same purpose to prevent ginger
oil from evaporating. In the refining process, fine ginger powder has a large
surface area, making it easier for a solvent to dissolve the ginger oil
component more quickly.
5. What the fuction of Na2SO4 in this experiment?
 as a drying agent used to absorb the remaining water content in the oil
6. Mention at least five compounds contained in the essential oil of ginger and
write down the structure formula!

Compounds (Presentage) Structure

Geraniol (25.9%)

a-zingiberen (9,5%)

(E,E)-a-farnesen (7,6%)

Neral (7,6%)

ar-curcumen (6,6%)

β-sesquiphellandren
(27,16%)

Caryophyllen (15,29%)

β-bisabolen (11,4%)
II. Calculate
1. Rendement mass of Ginger Oil :
Mass of experiment = 1,4 grams
Mass of ginger = 10 grams

𝑚𝑎𝑠𝑠 𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡
Mass rendement = x 100%
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑔𝑖𝑛𝑔𝑒𝑟
1,4 𝑔𝑟𝑎𝑚𝑠
= x 100%
10 𝑔𝑟𝑎𝑚𝑠

= 14%

2. Mass of Water
Mass wet ginger = 1 grams
Mass dry ginger = 0,4 grams
Mass of water = 0,6 grams
0,6 𝑔𝑟𝑎𝑚𝑠
Precentage of water = x 100%
1 𝑔𝑟𝑎𝑚𝑠

= 60%
III. Documentation

packed ginger by filter paper

with up and down bonded set soxhlet and reflux before extracted

the result of ginger oil after

after extracted filtered the result
extracted

set at evaporator test the index bias of ginger oil the result of ginger oil