FLAVOUR AND FRAGRANCE JOURNAL

Flavour Fragr. J. 2002; 17: 136–140

DOI: 10.1002/ffj.1052

Essential oil composition of Damask rose (Rosa

damascena Mill.) distilled under different pressures and
temperatures†
Kiran G. D. Babu,1Ł Bikram Singh,1 Virendra P. Joshi2 and Virendra Singh1
1 NPP Division, Institute of Himalayan Bioresource Technology, Post Box 6, Palampur (HP)–176 061, India
2 Promotive Health Care Pvt. Ltd, Dalmia Industries, Hotel Highway Home, Chamba Ghat, Solan (HP), India
Received 13 March 2001
Revised 3 July 2001
Accepted 23 July 2001

ABSTRACT: Experiments were conducted on field distillation unit to distil rose oil and rose water from the
fresh flowers of Damask rose (Rosa damascena Mill.) under different pressures and temperatures to study and
compare the essential oil composition by GC–FID. The monoterpene hydrocarbons and esters were found to be
in traces, and stearoptene content was found to be higher in the oil distilled under high pressure, as compared to
oil produced under atmospheric pressure. In general, the percentage of total alcohols (55.25–83.41%) in rose oil
increased with the increase in pressure and temperature of the distillation. Physicochemical properties of rose oil
distilled at varying level of temperatures and pressures are discussed. A comparative study was also conducted
of rose oil constituents from dichloromethane-extracted rose water and redistilled rose water under atmospheric
and higher pressure. At higher pressure early-eluting components in the GC column were present in traces and
decrease in total alcoholic content was observed. It can be concluded that distillation conducted under pressure
does not yield good quality oil. However, dichloromethane-extracted rose oil from rose water carries a higher
amount of 2-phenylethyl alcohol. The total rose alcohol content present in rose water was higher than in rose oil.
Copyright  2002 John Wiley & Sons, Ltd.
KEY WORDS: Rosa damascena; Damask rose oil; rose water; high pressure distillation; essential oil composition;
extraction; dichloromethane

Introduction or redistillation of the first distillate. Certain plant mate-

There are different kinds of traditional and modern
devices for the distillation of rose oil.1,2 A good num-
ber of reports have appeared on the chemical evaluation
of rose oil around the world.3 – 6 Exhaustive reviews
have been published from time to time by Lawrence.7,8
Plant-derived essential oils are not the true-to-type nat-
ural compounds as present in living plants, but complex
artefact products developed during the water-distillation
process, due to the influence of higher temperature,
pH change, etc., inside the distillation stills. Decom-
position products formed by over-heating of the plant
charge are reported as H2 S, NH3 , CH3 OH, CH3 COOH,
CH3 COCH3 and CH3 CHO, which are partially soluble in
water and dissolve in the distillation water.9 For this rea-
son, redistilled distillate (second distillation water) can
have an unpleasant odour, due to the repeated distillation
rials, such as orris root, sandalwood, clove, caraway seed
and pine needles, are occasionally distilled with steam
of a pressure higher than atmospheric in order to obtain
a more favourable ratio of oil to water in the distillate,10
i.e. to shorten the length of distillation and to increase
the total yield of oil. When distillation is carried out
under pressure, the density of steam and the tempera-
ture gradient between the general vapour space and the
point of evaporation of the oil on the herb surface also
increases,11 which helps in reducing distillation time as
the rate of evaporation of oil increases with the rise of
pressure. The increase in steam density, due to increase
in pressure inside the still, means the mass of steam
per unit volume plant charge is increased. The relation
between pressure and density of the steam was correlated
by the following equation:12
P / 2/3

where P is the mass of steam in contact with given heat

*Correspondence to: K. G. D. Babu, NPP Division, Institute of Hima- transfer area and  is the mass of steam per unit volume.
layan Bioresource Technology, Post Box 6, Palampur (HP)–176 061,
India. E-mail: gdkiranbabu@rediffmail.com The effect of high pressure appears to be more use-
† IHBT Publication No. 9907. ful to recover oil from the spent material/charge when

Copyright  2002 John Wiley & Sons, Ltd.


the plant material has not been distilled properly in a
previous batch of distillation at atmospheric pressure.9
The oil distilled under pressure possesses a darker
colour, which may be due to thermal decomposition or
the presence of metals or fine plant dust carried over
by the steam, especially when the live steam enters
the still with force. When steam is injected at lower
rates, the plant charge becomes somewhat wet by steam
condensation, and the dust particles are retained by the
plant material. Water distillation of plant material at high
pressure is not advisable because the resulting higher
temperature gives rise to the decomposition of prod-
ucts which impart a disagreeable ‘burnt’ note to the
oil. Aromatic herbs containing oils having high boiling
constituents are chemically stable at higher temperature,
e.g. 2-phenylethyl alcohol (b.p. 222.02 ° C at 760 mmHg)
and linalool (b.p. 198.3 ° C at 760 mmHg), associated
with high-pressure distillation, are best distilled at rela-
tively higher pressures.9 The variation in chemical and
sensory properties of rose oil extracted by supercritical
carbon dioxide and hydrodistillation has been studied by
Boelens.13 The objective of the present study is focused
on the evaluation of chemical and physical properties of
rose oil distilled at different pressures and temperatures.
To the best of our knowledge, no such studies have been
reported in the literature until now.
Experimental
Plant Material
Damask rose (Rosa damascena Mill.) is cultivated at
an elevation of 1475 m msl, (32.6 ° N, 76.18 ° E) at the
Institute’s farm, situated in the mid-hills of the west-
ern Himalayas (Dhauladhar range). The flowers were
plucked early in the morning before sunrise during the
months of April–May and utilized for distillation.
Distillation
A direct-fired field distillation unit containing a distilla-
tion tank (Capacity, 300 l), a cohobation column, con-
denser and the receiver, all made up of stainless steel,
which can process 35–40 kg fresh rose flowers/batch,
was installed at our Institute farm at an altitude of
1475 m msl (atmospheric pressure, 638.57 mmHg; boil-
ing point of water, 96 ° C). Fresh rose flowers (35 kg)
were charged into the distillation unit along with 100 l
fresh water. The unit was heated by direct firing of
agrowaste and the rose oil distilled under pressure. In
the beginning the whole system was kept open to atmo-
spheric pressure until the temperature rose to 70 ° C, and
consequently the air present in the unit was replaced by
the vapour. After complete removal of air from the unit,
Copyright  2002 John Wiley & Sons, Ltd.
ESSENTIAL OIL OF ROSA DAMASCENA 137
the air vent was closed and the whole unit was operated
as a closed system to distil the flower oil under differ-
ent pressures. Three batches of fresh rose flowers were
distilled at 0.21, 0.42, 0.58 and 0.8 kg/cm2 gauge pres-
sure at corresponding temperatures of 105, 110, 114 and
117 ° C, respectively, and average values were taken. The
pressure, temperature and rate of distillation were con-
trolled manually. The vapours produced in the still were
cohobated in a cohobation column and condensed in a
receiver equipped with cold water circulation. The pro-
cess was completed after collection of 25 l distillate at
an average rate of 116 ml/min. The same procedure was
followed when oil was distilled at ambient temperature
and pressure, except that the air vent was kept opened
to maintain the atmospheric pressure and the vapours
were condensed in a shell and tube condenser and 40 l
of distillate was collected. Three batches of fresh flow-
ers were distilled at normal atmospheric pressure. The
oil collected in the receiver was separated from the rose
water and dried over anhydrous Na2 SO4 . The average oil
compositions distilled at different pressures and temper-
atures, along with their standard deviations, are shown
in Table 1.
Solvent Extraction of Rose Oil from Rose Water
Rose water collected in the receiver, distilled under
pressure and at ambient temperature and pressure in
this semi-pilot plant was extracted with dichloromethane
(DCM), dried over anhydrous Na2 SO4 , filtered and then
distilled in vacuo at 40 ° C.
Extraction of Rose Oil from Rose Water by
Redistillation
Rose water collected in receiver, distilled under pressure
and at ambient temperature and pressure, was redistilled
in Clevenger-type apparatus14 to separate the oil. The
redistilled rose oil was dried over anhydrous Na2 SO4 .
The oil samples were analysed by GC–FID.
Analysis
GC analysis of the oil samples was performed on Shi-
mazdu Gas Chromatograph GC-14B, using nitrogen as
a carrier gas with a flow rate 40 ml/min, equipped with
FID and C-R7A Chromatopac printer and fitted with a
SE-30 column, 30 m ð 0.25 mm i.d. Temperature pro-
gramme was 40–200 ° C at 10 ° C/min, held for 2 min
at 40 ° C and for 15 min at 200 ° C. Sample injection
and detector temperatures were kept at 250 and 230 ° C,
respectively.
GC–MS analysis was conducted on Perkin-Elmer 910
model equipped with SE-30 column, 30 m ð 0.25 mm
Flavour Fragr. J. 2002; 17: 136–140
138 K. G. D. BABU ET AL.

Table 1. Comparative chemical composition (%) of rose oil distilled at different temperatures and pressures

Constituents Temperatures (° C)
96 105 110 114 117
˛-Pinene 1.15 (0.13) tr — 1.00 (0.82) 0.35 (0.12)
Sabinene 0.11 (0.03) — — — tr
Myrcene 0.25 (0.25) — — 0.14 (0.12) tr
ˇ-Pinene 0.63 (0.15) 0.18 (0.04) tr 0.37 (0.12) 0.22 (0.12)
2-Phenylethyl alcohol 4.32 (0.69) 3.80 (0.70) 9.63 (0.55) 9.08 (4.68) 7.63 (1.12)
Linalool 0.81 (0.20) — — — 2.17 (1.58)
cis-Rose oxide 0.19 (0.02) tr tr tr 0.12 (0.03)
trans-Rose oxide 0.10 (0.02) — — — tr
Terpinen-4-ol 0.19 (0.03) tr 0.30 (0.09) 0.12 (0.08) 0.24 (0.12)
˛-Terpineol 0.86 (0.36) 0.55 (0.39) 2.71(0.69) 1.82 (0.78) 2.22 (0.35)
Citronellol C Nerol 35.14 (1.75) 27.83 (0.21) 32.08 (1.23) 33.59 (3.12) 38.63 (1.48)
Geraniol 21.33 (2.00) 15.37 (0.21) 17.43 (1.42) 19.53 (3.62) 26.50 (2.74)
Eugenol 2.04 (0.20) 1.86 (0.74) 1.56 (1.31) 2.02 (0.30) 3.34 (0.48)
Damascone 0.29 (0.32) 0.25 (0.21) 0.31 (0.29) 0.39 (0.38) 0.25 (0.22)
Geranyl acetate 3.22 (0.63) 3.84 (0.84) 4.08 (1.96) 3.61 (0.45) 2.56 (0.48)
ˇ-Ionone 0.20 (0.09) tr tr tr tr
Methyl eugenol 0.72 (0.08) 0.41 (0.27) 0.68 (0.15) 0.77 (0.05) 1.13 (0.37)
ˇ-Bourbonene 1.05 (0.22) 1.21 (0.63) 0.57 (0.14) 0.49 (0.10) 0.45 (0.38)
ˇ-Elemene 0.56 (0.11) 0.66 (0.04) 0.18 (0.06) 0.16 (0.25) 0.19 (0.01)
ˇ-Caryophyllene 0.58 (0.13) 0.61 (0.09) 0.26 (0.05) 0.19 (0.08) 0.19 (0.06)
˛-Humulene 1.00 (0.29) 0.55 (0.15) 0.39 (0.13) 0.44 (0.05) 0.28 (0.17)
˛-Cadinene 0.39 (0.08) 0.59 (0.19) 0.50 (0.13) 0.37 (0.06) 0.15 (0.24)
Docosane 0.40 (0.21) 0.52 (0.28) tr 0.10 (0.25) 0.17 (0.05)
Heptadecane 3.31 (1.83) 6.02 (0.03) 5.11 (1.12) 2.58 (0.91) 1.42 (0.91)
FarnesolŁ 2.72 (1.23) 5.43 (0.47) 3.06 (0.62) 2.23 (0.92) 1.55 (0.34)
9-EicoseneŁ 2.10 (0.32) 5.00 (0.27) 3.56 (1.41) 3.33 (1.31) 1.50 (0.36)
Nonadecane 15.42 (0.92) 24.67 (1.49) 17.28 (6.51) 17.38 (6.51) 7.28 (1.09)
Rose oxides 0.29 tr tr tr 0.12
Stearoptenes 21.23 36.21 25.95 23.39 10.37
Rose alcohols 68.13 55.25 67.45 69.16 83.41
Lower hydrocarbons C long chain estersŁŁ 2.59 0.18 tr 1.51 0.80
The data mentioned in the parenthesis are corresponding standard deviation (š) of the reading.
tr D trace (<0.1%).
Ł
Correct isomer not identified.
ŁŁ
Includes traces and unidentified constituents.

i.d., using the same conditions as in GC. Helium was
used as the carrier gas. Identification of constituents was
carried out with the help of retention times of standard
substances by comparison of mass spectra with the data
given in the literature,15 – 17 and the NIST library18 con-
tains approximately 54 000 compounds available with
software installed in the computer and our own created
library.
Results and Discussion
The composition of rose oil distilled at different tem-
peratures, i.e. at 105, 110, 114 and 117 ° C, correspond-
ingly at 0.21, 0.42, 0.58 and 0.8 kg/cm2 gauge pressures,
was compared with oil distilled at ambient temperature
and pressure and the data are shown in Table 1. With
slight increase in temperature (96 to 105 ° C) and pres-
sure (0.0 to 0.21 kg/cm2 gauge), the variation in content
of phenylethyl alcohol was not significant, but increased
by 123% with an increase in temperature to 110 ° C
and 0.42 kg/cm2 gauge pressure. Similarly, the linalool
was increased by 168% at 117 ° C and 0.8 kg/cm2 . This
increasing trend was also observed in citronellol C nerol
and geraniol concentration. In general, the rose alco-
hols increased from 55.25% to 83.41% with increase in
pressure and temperature. This could be due to the alco-
holic nature of the compounds, which are more soluble
and best distilled at higher pressures and temperatures.9
The oil distilled under pressure contains ˇ-ionone in
traces, whereas the oil distilled at atmospheric pres-
sure contains 0.20% of ˇ-ionone. Lower terpenes, long
chain esters and rose oxides are found in traces or in
lower concentrations in rose oil distilled under pressure
in comparison to the oil distilled at atmospheric pres-
sure. Sesquiterpene hydrocarbons content also decreased
with increase in temperature and pressure. The decrease
in lower terpenes, esters, rose oxides and sesquiterpene
hydrocarbons may be due to the decomposition of these
compounds at higher temperature and pressure.
The percentage of monoterpene hydrocarbons and
esters (2.59%) was higher in oil distilled at atmospheric
pressure. Stearoptene content decreased with increase in
pressure and temperature from 36.21% to 10.37%. Other
constituents remained almost unchanged. The colour of
the oil changed from transparent pale yellow to reddish

Copyright  2002 John Wiley & Sons, Ltd. Flavour Fragr. J. 2002; 17: 136–140
 ESSENTIAL OIL OF ROSA DAMASCENA 139

brown and then to dark brown as the temperature and oil distilled in copper-made country stills (Deg and
pressure increased. It was reported that the use of copper Bhapkas).1 The reason for the reddish tinge in rose oil
receivers imparts a reddish tinge to the rose oil, and may be due to distillation carried out under pressure.
rust-coloured sediments have often been noticed in rose Any increase in boiling point of a mixture paves the

Table 2. Differences in physicochemical properties of oil distilled under higher pressure and at normal atmospheric
pressure

S. No. Oil distilled under pressureŁ Oil distilled at atmospheric pressure

1. Reddish-brown to dark brown colour Transparent pale yellow colour
2. Rose characteristics with fresh, floral, light burning note, Fresh, rosaceous, pleasant, sweet, floral, green, herbaceous,
heavy, earthy odour light spicy odour
3. The oil content in the rose water is 0.07% on redistillation Rose water contains 0.03% oil on redistillation
4. Rose alcohols content increased with increase in pressure Rose alcohols content is around 68%
5. Stearoptene content decreased with increase of temperature Stearoptene content is 21.23%
6. Lower hydrocarbons present as traces Lower hydrocarbons are very well present
7. Specific gravity D 0.8653 Specific gravity D 0.8589
8. Refractive index D 1.4861 Refractive index D 1.4805
9. Optical rotation, [˛]D 22 ° C could not be determined Optical rotation, [˛]D 22 ° C D 1 ° 400
10. Acid value D 9.3466 Acid value D 7.8424
11. Ester number as geranyl acetate D 63.85 Ester number as geranyl acetate D 64.71
12. Miscibility: clearly soluble in 1.5–2 volumes of 90% Miscibility: clearly soluble in 1.0–1.5 volumes of 90%
alcohol alcohol
13. Congealing point D 20.0 ° C Congealing point D 18.5 ° C
Ł The oil distilled under different pressures, i.e. 0.21, 0.42, 0.58 and 0.8 kg/cm2 gauge pressures, correspondingly at 105, 110, 114 and 117 ° C, are pooled and then
the properties were evaluated.

Table 3. Comparative chemical composition (%) of rose oil extracted from rose water by dichloromethane (DCM)
and redistillation

Constituents Higher pressure Atmospheric pressure

Extracted Redistilled in Extracted Redistilled in
with DCMŁ Clevenger apparatus with DCMŁ Clevenger apparatus
˛-Pinene 0.37 0.10 tr —
Sabinene — tr 0.10 —
Myrcene — tr tr tr
ˇ-Pinene — tr tr 0.17
2-Phenylethyl alcohol 55.16 5.41 63.12 2.49
Linalool 7.93 10.98 6.62 23.04
cis-Rose oxide tr 0.18 tr 0.28
trans-Rose oxide tr tr tr tr
Terpinen-4-ol 0.31 0.71 0.24 0.77
˛-Terpineol 2.79 6.37 2.63 9.20
Citronellol C Nerol 13.02 32.40 11.05 34.89
Geraniol 12.23 31.09 8.56 21.30
Eugenol 3.47 4.20 3.52 2.79
Damascone 0.07 0.05 0.04 0.02
Geranyl acetate 0.15 0.54 0.34 —
ˇ-Ionone — — 0.037 0.02
Methyl eugenol 0.71 1.70 0.61 1.52
ˇ-Bourbonene — tr — —
ˇ-Elemene — tr — —
ˇ-Caryophyllene — tr — —
˛-Humulene — tr — —
˛-Cadinene — tr — —
Docosane — tr — —
Heptadecane 0.51 0.48 tr 1.87
FarnesolŁŁ — 0.45 — —
9-EicoseneŁŁ — 0.24 — —
Nonadecane tr 1.07 tr —
Rose oxides tr 0.21 tr 0.30
Stearoptenes 0.55 1.80 tr 1.87
Rose alcohols 95.62 93.31 96.35 96.00
Lower hydrocarbons C estersŁŁŁ 2.05 1.44 1.84 0.62
Ł DCM, dichloromethane.
tr D trace.
ŁŁ Correct isomer not identified.
ŁŁŁ
Includes traces and unidentified constituents.

Copyright  2002 John Wiley & Sons, Ltd. Flavour Fragr. J. 2002; 17: 136–140
140 K. G. D. BABU ET AL.
way for the formation of artefacts inside the still. Due
to the presence of these artefacts, the rose oil seems
to be reddish in colour. On further application of pres-
sure, the non-volatiles undergo more or less profound
decomposition, with accompanying formation of unde-
sirable volatile substances, which considerably impair
the colour and odour of the oil.9 The difference in some
of physicochemical properties of oil distilled under high
pressure and normal pressure are shown in Table 2. The
congealing point of oil distilled under pressure is 20 ° C,
whereas it is only 18.5 ° C in oil distilled at atmospheric
pressure. The optical rotation varied significantly for oils
distilled at normal and under higher pressure and temper-
ature. The optical rotation of the oil distilled at normal
atmospheric pressure was observed as ()1° 400 , whereas
the same could not be obtained for the oil distilled under
pressure, due to its dark brown colour. The deviation in
other physicochemical properties are not so significant.
All the properties were evaluated at room temperature
of 22 ° C.
A comparative study of rose oil constituents extracted
by dichloromethane from rose water and redistillation
of rose water under high and normal pressures was
also conducted. The application of higher pressure
and temperatures in distillation played an important
role in rose oil composition. The odour of rose
water distilled under pressure was mixed with ‘burnt
notes’, and rose oil chemical composition in rose
water at higher and normal pressures and temperatures
is given in Table 3. Dichloromethane extract of rose
water showed higher contents of 2-phenylethyl alcohol
(55.16%, 63.12%) and lower contents of citronellol C
nerol (13.02%, 11.05%), geraniol (12.23%, 8.56%)
and linalool (7.93%, 6.62%), as compared to lower
content of 2-phenylethyl alcohol (5.41%, 2.49%) and
higher content of citronellol C nerol (32.40%, 34.89%),
geraniol (31.09%, 21.30%) and linalool (10.98%,
23.04%) in redistilled rose water at higher and
atmospheric pressures, respectively. The total alcohols
were observed at higher levels in oil extracted and
Copyright  2002 John Wiley & Sons, Ltd.
redistilled from rose water (Table 3) than in rose oil
distilled directly from the flowers (Table 1).
Acknowledgements—The authors are grateful to the Director, IHBT
(CSIR), Palampur, for continuous encouragement.
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