OLEUM ROSÆ.

_Attar or Otto[997] of Rose_, _Rose Oil_; F. _Essence de Roses_; G.

_Rosenöl_.

=Botanical Origin=—_Rosa damascena_ Miller, var.—This is the rose

cultivated in Turkey for the production of attar of rose; it is a tall

shrub with semi-double, light-red (rarely white) flowers, of moderate

size, produced several on a branch, though not in clusters. Living

specimens sent by Baur[998] which flowered at Tübingen, were examined

by H. von Mohl and named as above.[999]

_R. damascena_ is unknown in a wild state. Koch[1000] asserts that

it was brought in remote times to Southern Italy, whence it spread

northward. In the opinion of Baker[1001] Rosa damascena is to be

referred to Rosa gallica (see p. 259 above); it must be granted that

the Rose mentioned in footnote 2, as grown with one of us, approaches

very much to Rosa gallica.

=History=—Much as roses were prized by the ancients, no preparation

such as rose water or attar of rose was obtained from them. The

liquid that bore the name of _Rose Oil_ (ῤόδινον ἔλαιον) is stated by

Dioscorides[1002] to be a fatty oil in which roses have been steeped.

In Europe a similar preparation was in use down to the last century,

_Oleum rosarum_, _rosatum_ or _rosaceum_, signifying an infusion of

roses in olive oil in the _London Pharmacopœia_ of 1721.

[997] _Attar_ or _Otto_ is from the word _itr_ signifying _perfume_ or

_odour_; the oil is called in Turkish _Itr-yàghi_ i.e. _Perfume-oil_,

and also _Ghyùl-yàghi_ i.e. _Rose oil_.

[998] A living plant followed by excellent herbarium specimens has been

kindly given to me by Dr. Baur of Blaubeuren, the father of Dr. Baur of

Constantinople—D. H.

[999] Wiggers u. Husemann, _Jahresbericht_ for 1867. 350.

[1000] _Dendrologie_, i. (1869) 250.

[1001] _Journ. of Botany_, Jan. 1875. 8.

[1002] Lib. i. c. 53.

The first allusion to the distillation of roses we have met with, is in

the writings of Joannes Actuarius,[1003] who was physician to the Greek

emperors at Constantinople towards the close of the 13th century. Rose

water was distilled at an early date in Persia; and Nisibin, a town

north-west of Mosul, was famous for it in the 14th century.[1004]

Kämpfer speaks[1005] with admiration of the roses he saw at Shiraz

(1683-4), and says that the water distilled from them is exported

to other parts of Persia, as well as to all India; and he adds as a

singular fact, that there separates from it a certain fat-like butter,

called _Ættr gyl_, of the most exquisite odour, and more valuable even

than gold. The commerce to India, though much declining, still exists;

and in the year 1872-73, 20,100 gallons of rose water, valued at 35,178

rupees (£3,517), were imported into Bombay from the Persian Gulf.[1006]

Rose oil itself is no longer exported from Persia, as it still used to

be from Shiraz in the time of Niebuhr (1778).

Rose water was much used in Europe during the middle ages, both in

cookery and at the table. In some parts of France, vassals were

compelled to furnish to their lords so many bushels of roses, which

were consumed in the distillation of rose water.[1007]

The fact that a butyraceous oil of delicious fragrance is separable

from rose water, was noticed by Geronimo Rossi[1008] of Ravenna in

1582 (or in 1574?) and by Giovanni Battista Porta[1009] of Naples in

1589; the latter in his work on distillation says—“Omnium difficillime

extractionis est rosarum oleum atque in minima quantitate sed

suavissimi odoris.”[1010] The oil was also known to the apothecaries

of Germany in the beginning of the 17th century, and is quoted in

official drug-tariffs of that time.[1011] Angelus Sala, about 1620, in

describing the distillation of the oil speaks of it as being of “ ...

candicante pinguedine instar Spermatis Ceti.” In Pomet’s time (1694) it

was sold in Paris, though, on account of its high price, only in very

small quantity. The mention of it by Homberg[1012] in 1700, and in a

memoir by Aublet[1013] (1775) respecting the distillation of roses in

the Isle of France, shows that the French perfumers of the last century

were not unacquainted with true rose oil, but that it was a rare and

very costly article.

The history of the discovery of the essence in India, is the subject

of an interesting and learned pamphlet by Langlès,[1014] published

in 1804. He tells us on the authority of oriental writers, how on

the occasion of the marriage of the Mogul emperor Jehan Ghir with

Nur-jehan, A.D. 1612, a canal in the garden of the palace was filled

with rose water, and that the princess observing a certain scum on the

surface, caused it to be collected and found it of admirable fragrance,

on which account it received the name of _Atar-jehanghiri_, i.e.

_perfume of Jehan Ghir_. In later times, Polier[1015] has shown that

rose oil is prepared in India by simple distillation of the flowers

with water. But this Indian oil has never been imported into Europe as

an article of trade.

[1003] “ ... stillatitii rosarum liquoris libra una.” _De Methodo

Medendi_, lib. v. c. 4.

[1004] _Voyage d’Ibn Batoutah_, trad. par Defrémery, ii. (1854) 140.

[1005] _Amœnitates_, 1712. 373.

[1006] _Statement of the Trade and Navigation of the Presidency of

Bombay_ for 1872-73, part ii. 52.

[1007] Le Grand d’Aussy, _Hist. de la vie privée des François_, ii.

(1815) 250.

[1008] Hieronymi Rubei Rav. _De Destillatione_, Ravennæ, 1582. 102.

[1009] _Magiæ Naturalis libri xx_, Neap. 1589. 188.

[1010] _De Distillatione_, Romæ (1608) 75.

[1011] Flückiger, _Documente zur Geschichte der Pharm._ Halle, 1876.

37. 38. 40.

[1012] _Observations sur les huiles des plantes—Mém. de l’Acad. des

Sciences_, 1700. 206.

[1013] _Hist. des Plantes de la Guiane françoise_, ii. Mémoires, p. 125.

[1014] _Recherches sur la découverie de l’Essence de Rose_, Paris, 1804.

[1015] _Asiatick Researches_, i. (1788) 332.

As already stated, the supplies at present come from European Turkey;

but at what period the cultivation of the rose and manufacture of its

oil were then introduced, is a question on which we are quite in the

dark. There is no mention of attar in the account given by Savary[1016]

in 1750 of the trade of Constantinople and Smyrna, but in the first

years of the present century some rose oil was obtained in the Island

of Chios as well as in Persia.[1017]

In English commerce, attar of rose was scarcely known until the

commencement of the present century. It was first included in the

British tariff in 1809, when the duty levied on it was 10_s._ per

ounce. In 1813 the duty was raised to 11_s._ 10½_d._; in 1819 it

was 6_s._, and in 1828, 2_s._ per ounce. In 1832 it was lowered to

1_s._ 4_d._ per lb., in 1842 to 1_s._ and in 1860 it was altogether

removed.[1018]

On searching a file of the _London Price Current_, the first mention of

“_Otto of Rose_” is in 1813, from which year it is regularly quoted.

The price (in bond) from 1813 to 1815, varied from £3 to £5 5_s._ per

ounce. The earliest notice of an importation is under date 1-8 July,

1813, when duty was paid on 232 ounces, shipped from Smyrna.

=Production=—The chief locality for attar of rose, and that by which

European commerce is almost exclusively supplied, is a small tract of

country on the southern side of the Balkan mountains, the “Tekne” of

Kazanlik or Kisanlik, an undulated plain famous for its beauty, as

picturesquely sketched by Kanitz[1019] and many other travellers. The

principal seat of the trade is the town of Kizanlik, in the valley of

the Tunja. The other important districts are those of Philippopli,

Eski Zaghra, Yeni Zaghra, Tchirpan, Giopca, Karadsuh-Dagh, Kojun-Tepe,

Pazandsik. North of the Balkans, there is only Travina to be mentioned

as likewise producing attar. All these places with Kizanlik were

estimated in 1859 to include 140 villages, having 2,500 stills.

The rose is cultivated by peasants in gardens and open fields, in

which it is planted in rows as hedges, 3 to 4 feet high. The best

localities are those occupying southern or south-eastern slopes.

Plantations in high mountainous situations generally yield less, and

the oil is of a quality that easily congeals. The flowers attain

perfection in April and May, and are gathered before sunrise; those

not wanted for immediate use are spread out in cellars, but are always

used for distilling the same day. The apparatus is a copper still of

the simplest description, connected with a straight tin tube, cooled

by being passed through a tub fed by a stream of water. The largest

establishment, “Fabrika,” at Kizanlik has 14 such stills. The charge

for a still is 25 to 50 lb. of roses, from which the calyces are not

removed. The first runnings are returned to the still; the second

portion, which is received in glass flasks, is kept at a temperature

not lower than 15° C. for a day or two, by which time most of the oil,

bright and fluid, will have risen to the surface. From this, it is

skimmed off by means of a small tin funnel having a fine orifice, and

provided with a long handle. There are usually several stills together.

[1016] _Dict. de Commerce_, iv. 548.

[1017] Oliver, _Voyage dans l’Empire Othoman_, etc. ii. (Paris, An 9)

139, v. (1807) 367.

[1018] Information obligingly communicated by Mr. Seldon of the

Statistical Office of the Custom-house.

[1019] _Donau-Bulgarien_, ii. (1877) 103-123.—A figure of a still is

given, p. 123. A good map of the Tekne of Kizanlik and environs will

be found in _Zeitschrift der Gesellschaft für Erdkunde zu Berlin_, xi.

(1876) Taf. 2.

The produce is extremely variable. According to Baur,[1020] whose

interesting account of attar of rose is that of an eye-witness, it

may be said to average 0·04 per cent. Another authority estimates the

average yield as 0·037 per cent.

The harvest during the five years 1867-71 was reckoned to average

somewhat below 400,000 _meticals_,[1021] or 4226 lb. avoirdupois; that

of 1873, which was good, was estimated at 500,000 _meticals_, value

about £70,000.[1022]

Roses are cultivated to a considerable extent about Grasse, Cannes

and Nice in the south of France; and besides much rose water, which

is largely exported to England, a little oil is produced. The latter,

which commands a high price, fuses less easily than the Turkish.

There is a large cultivation of the rose for the purpose of making

rose water and attar, at Ghazipur on the Ganges, Lahore, Amritsar

and other places in India, but the produce is wholly consumed in the

country. The species thus cultivated is stated by Brandis[1023] to be

_R. damascena_. Medinet Fayum, south-west of Cairo, supplies the great

demand of Egypt for rose vinegar and rose water.

Tunis has also some celebrity for similar products, which however do

not reach Europe. A recent traveller[1024] states that the rose grown

there, and from which attar is obtained, is _Rosa canina_ L., which

is extremely fragrant; 30 lb. of the flowers afford about 1½ drachms,

worth 15_s._ When at Genoa, in 1874, one of us (F.) had the opportunity

of ascertaining that excellent oil of rose is occasionally imported

there from Tunis.

The butyraceous oil which may be collected in distilling roses in

England for rose water is of no value as a perfume.

=Description=—Oil of rose is a light yellow liquid, of sp. gr. 0·87

to 0·89. By a reduction of temperature, it concretes owing to the

separation of light, brilliant, platy crystals of a stearoptene, the

proportion of which differs with the country in which the roses have

been grown, the state of the weather during which the flowers were

gathered, and other circumstances less well ascertained. The oil

produced in the Balkans solidifies, according to Baur, at from 11

to 16° C. In some experiments made by one of us[1025] in 1859, the

_fusing_ point of true Turkish attar was found to vary from 16 to 18°;

that of a sample from India was 20° C.; of oil distilled in the south

of France, 21 to 23°, of an oil produced in Paris, 29°; of oil obtained

in distilling roses for rose water in London, 30 to 32° C.

[1020] _Pharm. Journ._ ix. (1868) 286.

[1021] _Consular Reports presented to Parliament, May_, 1872.—The

_metical_, _miskal_ or _midkal_ is equal to about 3 dwt. troy=4794

grammes.

[1022] _Consular Reports presented to Parliament_, Aug. 1873. 1090.

[1023] _Forest Flora of North-western and Central India_, 1874. 200.—D.

Forbes Watson, Catal. of the Indian Department, Vienna exhibition,

1873. 98.

[1024] Von Maltzan, _Reise in den Regentschaften Tunis und Tripolis_,

Leipzig, 1870.

[1025] Hanbury, _Pharm. Journ._ xviii. (1859). 504-509. _Science

Papers_, 172.

From these data, it appears that a cool northern climate is not

conducive to the production of a highly odorous oil; and even in

Bulgaria experience shows that the oil of the mountain districts holds

a larger proportion of stearoptene than that of the lowlands.

Turkish oil of rose is stated by Baur to deviate a ray of polarized

light 4° to the right, when examined in a column of 100 mm. The oil

from English roses which we examined exhibited no rotation.

=Chemical Composition=—Rose oil is a mixture of a liquid constituent

containing oxygen, to which it owes its perfume, and the solid

hydrocarbon or stearoptene already mentioned, which is entirely

destitute of odour. The proportion which these bodies bear to each

other is extremely variable. From the Turkish oil, it may be obtained

to the extent of 18 per cent., and from French and English to 35, 42,

60 or even 68 per cent.

Though the stearoptene can be entirely freed from the oxygenated

oil, no method is known for the complete isolation of the latter. As

obtained by Gladstone[1026], it had a sp. gr. of 0·881 and a boiling

point of 216° C.

With regard to the stearoptene of rose oil, the analyses of Théodore de

Saussure (1820) and Blanchet (1833) long since showed its composition

to accord with the formula CₙH₂ₙ. The experiments of one of us[1027]

confirm this striking fact, which assigns to the stearoptene in

question a very exceptional place among the hydrocarbons of volatile

oils, all of which are less rich in hydrogen.

Rose stearoptene separates when attar of roses is mixed with alcohol.

We have isolated it also from oil obtained from Mitcham roses, by

diluting the oil with a little chloroform and precipitating with

glacial acetic acid or spirit of wine, the process being several times

repeated. The stearoptene was lastly maintained for some days at

100° C.; thus obtained, it is inodorous, but when heated evolves an

offensive smell like that of heated wax or fat. At 32·5° it melts; at

150° vapour is evolved; at 272° C. it begins to boil, soon after which

it turns brown and then blackish. Stains of the stearoptene on paper

do not disappear by the heat of the water-bath and the relapse of some

days.

If cautiously melted by the warmth of the sun, the stearoptene forms

on cooling microscopic crystals of very peculiar shape. Most of them

have the form of truncated hexahedral pyramids, not however belonging

to the rhombohedric system, as the angles are evidently not equal;

many of them are oddly curved, thus §. Examined under the polarizing

microscope, these crystals from their refractive power make a brilliant

object.

Rose stearoptene is a very stable body, yet by boiling it for some days

with fuming nitric acid, it is slowly dissolved, and converted into

various acids of the homologous series of fatty acids, and into oxalic

acid. Among the former, we detected butyric and valerianic. The chief

product is however succinic acid, which we obtained in pure crystals,

showing all the well-known reactions.

[1026] _Journ. of Chem. Soc._ x. (1872) 12.

[1027] Flückiger, _Pharm. Journ._ x. (1869) 147.

The same products are obtained even much easier by treating paraffin

with nitric acid; it yields however less of succinic acid. The general

behaviour and appearance of paraffin is in fact nearly the same as

that of rose stearoptene. But what is called _paraffin_, is a series

of extremely similar hydrocarbons, answering to the general formula

CₙH₍₂ₙ₊₂₎ (_n_ being equal to more than 16), the separation of which

has not yet been thoroughly effected. The fusion point of the different

kinds of paraffin generally ranges from 42 to 60° C., yet one sort from

the bituminous shale of Autun, prepared and examined by Laurent,[1028]

melts at 33° C., and in this respect agrees with our stearoptene. It

is therefore possible that the latter actually belongs to the paraffin

series.

We have not ascertained the correctness of Baur’s strange experiments

(1872, _Jahresbericht der Pharm._ p. 460), by which he believes to have

converted the liquid part of rose oil into the stearoptene by means of

a current of hydrogen.

=Commerce=—Formerly attar of rose came into commerce by way of

Austria; it is now shipped from Constantinople. From the interior,

it is transported in flattened round tin bottles called _kunkumas_,

holding from 1 to 10 lb., which are sewed up in white woollen cloth.

These sometimes reach this country, but more commonly the attar is

transferred at Constantinople to small white glass bottles, ornamented

with gilding, imported from Germany.

=Uses=—Attar of rose is of no medicinal importance, but serves

occasionally as a scent for ointments. Rose water is sometimes made

with it, but is not so good as that distilled from the flowers. Attar

is much used in perfumery, but still more in the scenting of snuff.

=Adulteration=—No drug is more subject than attar of rose to

adulteration, which is principally effected by the addition of the

volatile oil of an Indian grass, _Andropogon Schœnanthus_ L. This

oil, which is called in Turkish _Idris yàghi_, and also _Entershah_,

and is more or less known to Europeans as _Geranium Oil_, is imported

into Turkey for this express purpose, and even submitted to a sort

of purification before being used.[1029] It was formerly added to

the attar only in Constantinople, but now the mixing takes place

at the seat of the manufacture. It is said that in many places the

roses are absolutely sprinkled with it before being placed in the

still. As grass oil does not solidify by cold, its admixture with

rose oil renders the latter less disposed to crystallize. Hence

arises a preference among the dealers in Turkey for attar of the

mountain districts, which, having a good proportion of stearoptene,

will bear the larger dilution with grass oil without its tendency to

crystallize becoming suspiciously small. Thus, in the circular of a

commercial house in Constantinople, dated from Kizanlik, occur the

phrases—“_Extra strong oil_,”—“_Good strong congealing oil_,”—“_Strong

good freezing oil_;”—while the 3rd quality of attar is spoken of as

a “_not congealing oil_.” The same circular states the belief of the

writers, that in the season in which they wrote, “_not a single metical

of unadulterated oil_” would be sent away.

The chief criteria, according to Baur, for the purity of rose oil

are:—1. _Temperature at which crystallization takes place_: a good

oil should congeal well in five minutes at a temperature of 12·5° C.

2. _Manner of crystallizing._—The crystals should be light, feathery,

shining plates, filling the whole liquid. Spermaceti, which has been

sometimes used to replace the stearoptene, is liable to settle down in

a _solid cake_, and is easily recognizable. Furthermore, it melts at

50° C. and so do most varieties of paraffin. The microscopic crystals

of the latter are somewhat similar to those of rose stearoptene, yet

they may be distinguished by an attentive comparative examination.

[1028] _Ann. de Chim. et de Phys._ liv. (1833) 394.

[1029] For particulars, see Baur (p. 262, note 3).

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