As a rule, however, it consists of a mixture of musk substance taken
from good sacs which present a bad appearance, or have been torn, and
from sacs of an inferior quality, frequently adulterated with foreign
substances, such as dried blood, dung of birds, weathered bicarbonate
of soda, etc.
To open a musk sac, cut it with a sharp penknife around where the
hairless side joints the hairy side, and empty it by scraping it out
upon a sheet of paper. The membranes and hair are then removed by means
of pincers.
The musk-substance of the Tonkin sacs is generally a heavy, dry-feeling
mass; it is partially intermingled with and partially enveloped by
small, thin, soft, brown, somewhat transparent membranes and frequently
mixed with small hair. It is partially loose and crummy, and partially
consists of various lumps or grains of the size of a mustard seed to
that of a pea, which are more or less roundish, more seldom angular,
softer or harder (but can always be readily cut), of a fatty lustre and
black-brown or dark-red color. In fresh sacs, the mass is frequently
soft, and, when bruised, somewhat smeary, but never unctuous. On
rubbing, it becomes paler in color, and glistening hair-like, paler,
gray or whitishyellow particles, sometimes of a crystalline texture,
appear. The odor of the musk substance is peculiar, strong, and very
constant; it is agreeable only when much diluted.
Musk is not a substance of a constant chemical and physical
constitution, the reason for this being found in the age and the
different foods of the musk animal, the season in which it is killed,
and the degree of dryness of the musk-substance. Water dissolves ¾
of good musk and 90 per cent. alcohol ½. The alcoholic solution is
not precipitated by water. Musk further contains fat-like substances,
wax, gall-substances (together 10 to 12 per cent.), glue-substances
and albumen (6 to 9 per cent.), traces of lactic and butyric acids,
phosphates, sulphates and hydrochlorates of the alkalies and alkaline
earths, frequently strong traces of ammonium carbonate and a volatile
oil, further moisture, humus-substance, and fibrous matter.
Musk, when dried, has a weak odor, which gradually becomes stronger on
moistening. There are several substances which destroy the musk odor,
especially bitter almonds, camphor, sulphur, acids and sulphates. The
odor adhering to a mortar in which musk has been rubbed can best be
removed by pounding bitter almonds in it.
Since, on account of the high price of musk, the musk animal is much
hunted, there is a possibility of it becoming in time extinct. For this
reason a substitute has been long searched for, and is believed to have
been found, especially, in the American musk-rat (_Fiber zibethicus_),
which is chiefly hunted for its skin. In this animal the musk is found
in two small sacs located between the anus and generative organs,
and is emitted when the animal becomes excited. According to R. S.
Cristiani, this musk is invaluable for the toilet soap industry of
America, it being nearly as good and strong as genuine musk. Cristiani
has formerly used much of it for scenting soaps, powders, etc., but
does not recommend it for essences. When used for soaps, some time is
required for the odor to become refined, and if a piece of soap scented
with it is stored for a few months, it would, according to Cristiani's
assertion, be difficult even for an expert perfumer to distinguish the
odor from that of genuine Tonkin musk.
As possible substitutes for the musk deer may further be mentioned
a species of rat indigenous to the West Indies, and an antelope of
North Africa. It is also said that musk derived from the Mississippi
alligator has been brought into commerce. The sacs are said to
be small, the odor somewhat different from that of genuine musk,
resembling that of civet, but suitable for perfuming purposes.
A process for the preparation of _artificial musk_ has been patented
by Dr. Baur, of Gispersleben. According to the specification, toluol
is mixed with the halogen compounds of butane and boiled with the
addition of aluminium chloride or aluminium bromide. The product of the
reaction is mixed with water and distilled with steam. The fraction
passing over between 338° and 392° F. is caught and treated with fuming
nitric acid and fuming sulphuric acid. The product obtained is washed
with water and alcohol, and crystallized. The artificial musk forms an
amorphous white powder, which in time becomes yellow. It is readily
soluble in 90 per cent. alcohol, but from solutions in weaker alcohol
it again crystallizes out at a cool temperature. The odor becomes very
pronounced after the addition of 5 drops of ammonia to 1 pound of a one
per cent. solution.
This artificial product having been in existence but for a short
time, it is not possible to come to a final conclusion as to its
availability. However, its odor differs essentially from that of the
genuine article, and it can scarcely be employed for fine extracts;
if low enough in price it might, however, be suitable for soaps and
cheaper perfumes.
Musk is very much adulterated, the Chinese being adepts in this
sophistication. Dried blood, on account of its resemblance to musk,
is among the most common adulterations, but, besides this, sand, iron
filings, hair, the dung of birds, wax, asphaltum, and many other
substances are introduced. They are mixed with a small portion of
musk, the powerful odor of which is communicated to the entire mass,
and renders the discovery of the fraud sometimes difficult. The bags
containing the musk should have the characteristics before described
as belonging to the natural sac, and present no sign of having been
opened. One of the grossest frauds, which is also perpetrated in
Europe, consists, according to Hager, in perforating the musk sac with
a needle, placing it in strong rum or weak spirit of wine, and, after
pressing it with the fingers, washing with spirit of wine and drying
in the air. By this means a tincture suitable for perfuming purposes
is obtained, while the musk-substance is increased in weight by the
absorption of moisture. Sacs thus treated are, however, readily
recognized, they being, after drying, gnarled and uneven.
Good musk-sacs should yield from 50 to 60 per cent. of musk. An
admixture of blood is detected by the musk acquiring a putrid odor
when moistened with water. The presence of pieces of metal, pebbles,
resin, etc., is recognized by the naked eye or with the assistance of
a magnifying glass. The microscope reveals, in pure musk, white and
brownish, irregularly-formed grains, cells, oil drops, and, generally,
also fungoid threads. Genuine musk burns with a white flame and leaves
a gray ash, which should not amount to more than from 5 to 8 per cent.
In perfumery musk is used for soap, sachet powders, and extracts. By
itself it is, however, scarcely employed, not even for the so-called
musk soaps or musk extracts. It is chiefly valued by the perfumer for
its property of rendering other perfumes used in combination with it
more durable and bringing out their scent. For scenting soaps the
musk must first be prepared. If to be used for milled soaps, it is
triturated in a mortar with clear sugar, while for cold stirred soaps,
weak potash lye of at the utmost 3° to 5° Bé. is poured over it. Weak
lye makes the odor more pronounced, while strong lye destroys it.
_Civet_ (_zibethum_) is derived from two animals of the genus
_Viverra_. The actual civet cat (_Viverra civetta, L._) lives in the
hottest parts of Africa from the Guinea Coast and the Senegal to
Abyssinia, where it is carefully bred for its civet. The product is
also obtained from _Viverra zibetha, L._, indigenous to the Moluccas
and Philippines. The civet is secreted in a cavity between the anus
and the external genitals, and is scraped out with a spoon. It is
semi-liquid, unctuous, yellowish, becoming brown and thicker by
exposure to the air, of a bitter, disagreeable, fatty taste, and of a
peculiar, urinose, disagreeable odor, resembling that of musk which
becomes agreeable only when much diluted and mixed with other perfumes.
When ignited it burns with a bright flame, leaving behind 3 to 4 per
cent. of ash. It is insoluble in water; in spirit of wine it partially
dissolves with difficulty, and with greater ease in warm ether and in
chloroform. It should form a homogeneous, non-crumbling mass. According
to M. Boutron Chalard, it contains free ammonia, stearin, olein, mucus,
resin, a yellow coloring substance, salts, and a volatile oil, the
latter giving the odor to it. In perfumery, civet is chiefly used as an
addition to other perfumes in order to strengthen them and make them
more constant. It is also employed for perfuming fine leather articles.
_Castor_ or _castoreum_ is a peculiar concrete substance obtained
from _Castor fiber_ or the beaver. In both sexes between the anus
and external genitals are two pear-shaped sac-like follicles (Fig.
24) united at their thin ends. The follicles contain, when fresh, a
semi-liquid substance which becomes more solid by drying. The castor
occurring in commerce is generally dried by smoke.
[Illustration: FIG. 24.]
In commerce two principal varieties are distinguished: Siberian or
Russian and Canadian, English or American castor, the first being the
most valuable. The length of a Siberian sac varies between 2.36 and
4.72 inches, the width between 0.98 and 2.55 inches, and the thickness
between 0.78 and 1.57 inches; it weighs from 1.76 to 8.81 ozs. One of
the sacs is generally somewhat smaller than the other. The exterior
skin of the sac is almost smooth and, in a dry state, dark brown; the
interior is dirty yellow, intermixed with a dense cellular tissue,
which envelops the castor-substance and is grown together with it. In a
dried state, the latter is dark brown, without lustre, almost friable,
of a very strong, peculiar odor, and a pungent, somewhat bitter,
aromatic taste.
The sacs of Canadian castor are smaller than the Siberian, they being
at the utmost 3.15 inches long, 0.98 inch thick, and darker and
uneven. The interior mass is resinous, hard, with a lustrous fracture,
red-brown, and can be readily pulverized. The odor is weaker, somewhat
musty and ammoniacal, and the taste more bitter and less pungent than
that of the Siberian castor.
Castor is much adulterated--pebbles, pieces of lead, dried blood,
etc., being frequently found in the sacs. These frauds can generally
be detected in cutting the sac open. Spurious sacs are said to be
frequently found among the genuine sacs of Canadian castor. These
spurious sacs are prepared by drying a mixture of castor, resin,
dragons' blood, etc., in the scrotum of goats.
In perfumery, castor is now very seldom used, the perfumers preferring
musk and civet, which, certainly, give a somewhat different scent.
_Ambergris_ is a fatty, waxy substance, often found floating on the sea
on the coasts of Arabia, Madagascar, Japan, etc. It is also found in
the cæcum of the sperm whale (_Physetus macrocephalus, Schow_), and
is supposed by some to be a morbid secretion in the urinary bladder.
According to Mr. Beale, it merely consists of the indurated fæces of
the animal, perhaps somewhat altered by disease. It has a gray-white
color, often with a black streak and a slight agreeable odor, like
that of benzoin, which becomes more pronounced on heating. When held
for some time in the hand it becomes soft and flexible. It melts at
the temperature of boiling water, and, when more strongly heated,
volatilizes in the form of a white vapor, leaving but slight traces
of ash behind. Its specific gravity is 0.8 to 0.9. It is insoluble in
water, sparingly soluble in cold spirit of wine, and more readily so
in hot spirit of wine, ether and volatile and fat oils. It is almost
completely soluble in absolute alcohol. Though ambergris crumbles
readily, it can only with difficulty be converted into coarse powder.
With the finger it can be polished like hard soda-soap.
The principal constituent of ambergris is ambrin or ambrein, a
non-saponifiable fat, which, from a saturated alcoholic solution of
ambergris, crystallizes, after standing for some time, in the form
of verrucose, whitish or lustrous acicular crystals. According to
John, ambergris consists of 85 per cent. ambrin, 12.5 per cent. sweet
balsamic extract, further benzoic acid, sodium chloride, and 1.5 per
cent. insoluble brown residue. When distilled with water, ambergris
yields 13 per cent. of a volatile oil having an agreeable odor. A
red-hot iron wire readily penetrates ambergris, and from the hole thus
made flows an oily liquid of a strong and agreeable odor.
On account of its high price, ambergris is frequently adulterated, the
commercial article being often nothing but an artificial mixture of
benzoin, olibanum, wax, and flour, with other substances, perfumed with
musk. Such adulterations are detected by the appearance, proportions
of solubility, nature of the fracture and the content of ash. A small
quantity of pure ambergris, exposed to heat, melts without forming
bubbles or scum. It is easily punctured with a heated needle, which,
when withdrawn, should come out clean and without anything adhering
to it, and the characteristic odor of ambergris should be immediately
evolved. The surface should be rugged, that with a smooth and uniform
surface being generally factitious.
In perfumery, ambergris is not so much used on account of its agreeable
odor, but rather to make the perfumes more constant.
CHAPTER VII.
ARTIFICIAL PERFUME-MATERIALS.
In speaking of the volatile oils used in perfumery, two artificial
perfume-materials, artificial oils of bitter almonds and wintergreen
have already been mentioned. There can be no doubt that when the
chemical construction of volatile oils is better known, chemistry
will succeed in preparing still more such combinations, valuable for
perfumery, or in converting cheap volatile oils into more valuable
ones, as has, for instance, been done by Bouchardat and Lafont, who
have successfully converted oil of turpentine into oil of lemons. These
chemists rectified French oil of turpentine at exactly 311° to 314.6°
F., dissolved in the distillate, which amounted to 120 grammes, an
equal quantity (120 grammes) of glacial acetic acid, cooled the mixture
and then carefully added, so that the temperature never exceeded 104°
F., 88 grammes of crystallized chromic acid dissolved in a sufficient
quantity of acetic acid. Notwithstanding that the greater portion of
the oil of turpentine remained unoxidized, a thorough reaction took
place, and the product of decomposition proved to be a hydrocarbon,
boiling at from 345.2° to 352.4° F., to which Bouchardat and Lafont
have applied the term "terpilene." The properties of this hydrocarbon,
especially its boiling point, corresponded with those of oil of lemons,
its odor also resembling that of the latter, but it contained about
one-sixth cymol which it was impossible to remove. Though thus far this
artificial oil of lemons is of no importance for perfumery, it is of
interest as showing the possibility of converting one volatile oil into
another.
The artificial musk, spoken of under "Musk," cannot be classed with the
previously-mentioned artificial perfumed-materials. The odoriferous
principle of the natural and artificial musk have nothing in common,
the odor depending not on a common chemical combination.
Besides the artificial perfume-materials already mentioned, but a
few others are employed in perfumery, viz: _Cumarin_, _heliotropin_,
_vanillin_, and _nitrobenzol_, or _oil of mirbane_. Another series of
artificial perfume-materials, the so-called fruit ethers, have also
been recommended for perfumery purposes. Although such products are
sometimes used, their employment is not advisable, since they produce
an irritating effect upon the bronchial tubes and respiratory organs,
and frequently cause headache.
_Cumarin._--The agreeable odor of new-mown hay is chiefly due to the
sweet-scented vernal grass (_Anthoxanthum odoratum, L._). This grass
contains an odoriferous substance, the _cumarin_. The latter is also
found in many other plants; for instance, in the tonka bean (the seeds
of _Dipterix odorata_), in the sweet woodruff (_Asperula odorata_),
and, combined with melilotic acid, in the melilot (_Melilotus
officinalis, Descr._).
Cumarin forms small, colorless crystals of a silky lustre. It is very
hard, cracks between the teeth, shows a smooth fracture, and sinks in
water. It has a very agreeable aromatic odor, which, on rubbing the
substance with the fingers, becomes like that of oil of bitter almonds,
and has a bitter, warm, and pungent taste. When pure it melts at 152.6°
F., but when containing fat, like that separated from tonka beans, at
from 104° to 122° F. Its boiling point lies at 554° F.; it volatilizes,
however, at far lower temperatures, diffusing an odor resembling that
of oil of bitter almonds, and sublimating in white needles. It is
soluble in alcohol, ether, acetic acid, fat, and volatile oils. Of cold
water (59° F.) 400 parts are, according to Buchner, required for its
solution, but of boiling water only 45 parts.
Tonka beans are the ripe seeds of _Dipterix odorata_. They are much
used in perfumery on account of their content of cumarin, and formerly
constituted the initial point for its manufacture. In commerce two
varieties are distinguished, viz., _Dutch tonka beans_, derived from
_Dipterix odorata, Willd._, indigenous to the forests of Guiana,
and _English tonka beans_, from _Dipterix oppositifolia, Willd._,
indigenous to Cayenne.
The Dutch tonka bean is 1.18 to 1.57 inches long, 0.39 to O.59 inch
wide, and O.27 to O.43 inch thick. It is generally slightly curved,
provided under the point with the hilum, and covered with a thin,
fragile, brown-black or black skin of a fatty lustre, upon which small
crystals of cumarin are generally found, so that it appears coated,
especially in the wrinkles, with a whitish dust. The kernel consists
of two yellow-brownish oleiferous catyledons, between which layers of
cumarin are generally found. The odor is agreeable, resembling that of
melilot, and the taste aromatic bitter. Dutch tonka beans contain fat,
sugar, malic acid, and malate of lime; further, starch, gum, and 1 to
5 per cent. of cumarin (C_{9}H_{6}O_{2}). The English tonka beans are
smaller, white-yellowish inside, nearly black outside, and of inferior
quality to the Dutch beans.
From tonka beans, cumarin may be obtained by two different methods.
One method consists in repeatedly extracting the bruised beans with
spirit of wine, distilling the latter off from the extract, and mixing
the residue with cold water, whereby cumarin contaminated with fat
is precipitated. To remove the fat, bring the whole to the boiling
point, filter the hot solution through a moist filter upon which the
fat is retained, and allow to cool, whereby the greater portion of the
cumarin crystallizes out; the remaining small portion is obtained by
evaporating the mother-lye.
According to the other method, the bruised tonka beans are distilled
with water. After 24 hours the greater portion of the cumarin separates
in a crystalline form. The residue remaining in solution can be
withdrawn from the water by shaking with petroleum-ether and subsequent
evaporation of the solvent. From one pound of good tonka beans, up to 4
drachms of cumarin may be obtained.
Cumarin is sometimes also obtained by purifying by recrystallization of
the débris found in the original boxes of tonka beans, which chiefly
consists of cumarin.
Perkin has recently succeeded in artificially preparing cumarin from
salicylic acid. By boiling the sodium salt of the latter in acetic
anhydride for a few minutes and then pouring into water, an oil-like
body is separated, whilst sodium acetate passes into solution. The
former is a mixture of acetic anhydride, salicylic acid and cumarin;
in distilling, the latter passes over last (at 554° F.), and congeals
in the receiver to a crystalline mass.
Cumarin is now synthetically prepared by several firms, that brought
into the market by Schimmel & Co., of Leipsic, especially being of
excellent quality. Although artificial cumarin is considerably lower
in price than that obtained from tonka beans, most perfumers still
prefer the extract from tonka beans prepared by themselves. There is,
however, no good reason for this, since a change in the respective
receipts for perfumes presents no difficulties, 8.46 drachms of cumarin
corresponding to 2.2 lbs. of best tonka beans.
_Heliotropin_ or _piperonal_ is of great importance in the manufacture
of perfumes. It forms small, colorless prismatic crystals, which have
an agreeable odor of héliotrope. Upon the tongue heliotropin produces
the same sensation as oil of peppermint under the same conditions, the
sensation being, however, more lasting. It melts at about 104° F., and
volatilizes at a higher temperature without leaving a residue. It is
soluble in alcohol and ether, and insoluble in cold water; in hot water
it melts to an oily liquid which floats upon the water.
Exposed to the action of heat and air, heliotropin acquires an uncomely
appearance, balls together and, under very unfavorable circumstances,
turns brown. It is then entirely decomposed and useless, and, hence,
should be kept in summer in as cool a place as possible. A temperature
of 95° F. has already an injurious effect upon the perfume, and it is
best not to buy it at all in the hot summer months. To preserve the
perfume in its entire freshness, it is advisable for consumers in hot
climates to at once dissolve the heliotropin in alcohol and to keep the
solution in a cool place.
Pepper serves as the initial point for heliotropin or piperonal, the
white variety being the best for the purpose. To obtain piperine,
contained in varying qualities (7 to 9 per cent.) in pepper, the
latter is repeatedly extracted with boiling alcohol. The extract is
then evaporated to one-third its volume, or the greater portion of the
alcohol is distilled off, and the resinous mass, obtained after the
addition of water, is repeatedly washed in water with the addition of a
small quantity of potash or soda lye, dissolved in alcohol and purified
by repeated recrystallization. To convert the white-yellow piperine
thus obtained into potassium piperate it is, together with equal
parts of potassium hydroxide and 5 to 6 parts of alcohol, kept gently
boiling for 24 hours in a well-closed flask provided with an ascending
Liebig cooler. A capacious flask should be used, as the mass pounds
quite vigorously. After cooling, the precipitate, which is obtained
in yellowish, lustrous lamina, is separated through a filter from the
dark-brown mother-lye, washed with cold alcohol and several times
recrystallized from hot water. A further discoloration may be effected
by the addition of animal charcoal.
The potassium piperate thus obtained forms nearly colorless prisms in
verucose groups, which, however, turn yellow when exposed to light.
By boiling the alcoholic mother-lye with ⅓ of the previously used
potash-lye, further small quantities of potassium piperate may be
obtained.
To obtain piperonal from the potassium piperate, dissolve 1 part of
the latter in 40 to 50 parts of hot water, and then slowly introduce,
with constant stirring, a solution of 2 parts potassium permanganate
in 50 parts of water. This precaution is absolutely necessary, as
otherwise the piperonal formed would be partially further oxidized and
lost. The paste-like mass formed is passed, while still hot, through a
straining cloth, and the residue repeatedly washed with boiling water
until it shows nothing more of the characteristic odor of héliotrope.
The wash-waters are combined with the first filtrate, and subjected to
distillation over a free fire.
The first distillates are richest in piperonal, it generally separating
already in the cooler. The fractionally caught distillate is allowed
to stand one or two days in as cool a place as possible, whereby the
greater portion of the piperonal separates in a crystalline form or in
fine lamina. To obtain the piperonal still remaining dissolved in the
water, the mother-lye, after the separation of the crystals through a
filter, may be repeatedly agitated with ether, whereby the piperonal
dissolves in the ether. The latter is carefully distilled off at as
low a temperature as possible (104° to 122° F.) in the water-bath or
allowed naturally to evaporate.
_Vanillin._--Vanilla is the not entirely ripe, pod-like, capsular
fruit (wrongly called pod), of a tropical orchid (_Vanilla planifolia,
Andrews_), which is cultivated in Mexico, the West Indies, and South
America. It is extensively used for flavoring, and its odoriferous
substance is highly valued in perfumery. The cross-section of the
capsule is thick and fleshy, filled with very small, black, lustrous
seeds stuck together by a gummy balsam with which they are coated. The
capsule has a sourish taste and has no value, the seeds, or rather
the balsam enveloping the seeds, being the substance on which the
odor and taste of vanilla depend. When the vanilla fruit becomes ripe,
the capsule opens and empties its content of seeds in the form of a
balsam-like mass.
The lustrous black-brown surface of vanilla is frequently coated with
white, delicate crystals, which were formerly taken for benzoic acid.
Bley and Vee first recognized them as a peculiar substance, which was
further examined by Gobley and Stokkebye. This substance, to which
Gobley applied the term _vanillin_, is the chief odoriferous substance
of vanilla. It is deposited upon the vanilla-crystals, when the latter
are densely and closely packed together and for some time exposed to
a heat of about 77° F. Of vanillin, vanilla contains 1.5 to 2.75 per
cent.; the Mexican variety containing 1.69 to 1.32 per cent., the
Bourbon No. I, 2.48 to 1.91 per cent., Bourbon No. II, 1.55 to 0.75 per
cent., and the Java, 2.75 to 1.56 per cent. It is singular, that the
highly valued Mexican vanilla has, generally speaking, a lower content
of vanillin than the other varieties.
At present, vanillin is prepared artificially. Tiemann and Harmann
first showed that by the oxidation of coniferin, a glucoside occurring
in the cambial sap of the _Coniferæ_, a product, perfectly identical
with the vanillin prepared from vanilla, is obtained. The coniferin
is obtained by barking the pine or silver fir, scraping together the
sap under the bark together with a portion of the liber and pouring
it into a vessel. The sap is then pressed off, boiled to separate
the albumin, filtered, evaporated to one-fifth its volume, and set
aside to crystallize. One hundred quarts of sap are said to yield
from 1 to 2 pounds of coniferin-crystals. By now allowing an aqueous
coniferin-solution to run into a heated mixture of 10 parts potassium
bichromate, 15 parts concentrated sulphuric acid, and 80 parts water,
and heating for 3 hours in a flask with back-flow cooler, a liquid
is obtained from which ether takes up a yellow oil. After treating
the latter with animal charcoal, dissolving in ether and evaporating
the latter, there remain colorless, acicular crystals of the odor and
taste of vanilla. These crystals consist of vanillin contaminated with
some vanillic acid. To separate the latter, purify with acid sodium
sulphite and recrystallize. After this operation, vanillin represents a
nearly white crystalline powder which melts at from 176° to 177.8° F.
In this form it is brought into commerce as a complete substitute for
vanilla, 5.64 drachms of it corresponding to about 1 pound of vanilla.
A medium-sized pine tree is said to yield vanillin of the value of 80
marks ($19.20).
Vanillin may also be prepared by oxidation from eugenol. Oil of cloves
is diluted with three times its volume of ether and agitated with
weak caustic potash solution to fix the eugenol on the potash. By
acidulating the alkaline solution and shaking with ether, the eugenol
is collected. After distilling off the ether, the eugenol is converted
with acetic anhydride into aceteugol, and the latter oxidized with
dilute, moderately-warmed potassium permanganate solution. The filtrate
is made slightly alkaline, concentrated, then compounded with acid and
the vanillin extracted with ether.
Vanillin (C_{8}H_{8}O_{3}) forms small colorless prisms of a strong
vanilla odor, a warm, vanilla taste, and an acid reaction. It is
readily soluble in hot water, alcohol, ether, chloroform, fat and
volatile oils, as well as in solutions of caustic alkalies and alkaline
carbonates. It melts when heated to from 176° to 177.8° F.; at a higher
temperature it sublimates without leaving a residue.
According to a notice published in the "Deutsch-Amerikanischen
Apotheker Zeitung," vanillin adulterated with benzoic acid has occurred
in the United States. A sample subjected to examination is said to
have been nothing but benzoic acid perfumed with vanillin. Such an
adulteration can be detected with the microscope, since vanillin
crystallizes in acicular crystals, and benzoic acid in lamina, which
can be readily recognized. Pure vanillin melts at 176° F., while
the melting points of such mixtures are considerably higher, it
being in one case at 249° F. By extracting such mixture with thin
sodium carbonate solution, benzoic acid passes into solution. After
neutralizing with hydrochloric acid, the filtrate yields with ferric
chloride a fawn-brown precipitate of ferric benzoate, and on adding
hydrochloric acid in excess, the benzoic acid, which dissolves
with great difficulty in cold water, is precipitated. By treating
the latter, or the ferric benzoate, with dilute sulphuric acid and
magnesium, the benzoic acid is reduced to benzaldehyde, which is
recognized by its characteristic odor of oil of bitter almonds.
_Nitrobenzol_ is obtained by treating benzol, or a mixture of it,
with toluol and their higher homologues, with strong nitric acid,
or a mixture of nitric and sulphuric acids, washing the product of
reaction with water and soda, caustic soda or ammonia, expelling the
unaltered hydrocarbons with steam and rectifying the residue. Three
varieties distinguished by their boiling points and odor occur in
commerce. The nitrobenzol or oil of mirbane (_essence de mirbane_) is
the so-called _light nitrobenzol_, which boils at from 401° to 415° F.
The _heavier_ varieties boil at a higher temperature and have a more or
less disagreeable odor; they are used in the manufacture of aniline and
aniline colors.
Pure oil of mirbane is pale yellow, the finest qualities being
colorless and almost as clear as water. It has an agreeable odor
resembling that of oil of bitter almonds, a specific gravity of 1.186
to 1.2 = 25° Bé., and congeals at 37.4° F. to a crystalline mass. It is
scarcely soluble in water, sparingly so in alcohol and with difficulty
in watery spirit of wine; it is miscible in all proportions with ether,
benzine, volatile oils, and most fat oils.
Oil of mirbane is largely manufactured in England, but the German
product is now generally preferred, it being purer and does not impart
to soap perfumed with it a yellowish tinge. The finest oil of mirbane
is prepared from pure crystallizable benzol, and again purified
by washing with potassium bichromate and sulphuric acid, and by
rectification with steam.
Pure nitrobenzol suffers no change by boiling with soda lye, while the
poorly rectified product colors the lye yellow or brown.
Nitrobenzol is frequently adulterated with spirit of wine, which is
recognized by shaking the oil with fat oil of almonds; in the presence
of spirit of wine a turbid mixture is formed. By shaking nitrobenzol
containing spirit of wine with an equal volume of water in a graduated
cylinder, its volume decreases.
Oil of mirbane is much used for perfuming soaps, but even the finest
quality of it cannot replace oil of bitter almonds for fine soaps
and perfumery. Great care has to be exercised in storing, as well
as in working, nitrobenzol, it igniting very readily, and it is
also poisonous. Even the vapors, when inhaled for some time, may
produce symptoms of poisoning, which consist in the skin acquiring a
leaden color, and heavy feelings in the limbs with cold extremities,
especially the hands and feet.
FRUIT ETHERS. At the London Exhibition, in 1851, various products
called apple oil, pear oil, pine-apple oil, etc., were shown. They were
examined by A. W. Hofmann, and found to consist of solutions of certain
ethers in alcohol. Since then the manufacture has greatly increased and
large quantities are now brought into commerce under the name of _fruit
ethers_ or _fruit essences_.
Fruit ethers are fluids possessing an agreeable, refreshing odor
closely resembling that of some fruits. For this reason they are
used in confectionery, in the manufacture of liqueurs and also as
a substitute for volatile oils, in the manufacture of perfumery.
Chemically, fruit ethers are combinations of an organic acid--acetic,
butyric, valerianic, etc.--with a so-called alcohol radicle, such as
ethyl and amyl. The preparation of fruit ethers being connected with
many difficulties, is seldom attempted by perfumers, especially as
products of an excellent quality can at a low rate be procured from
chemical laboratories making a specialty of their manufacture. However,
for the sake of completeness, a brief description of the fabrication of
the principal ethers used in their preparation shall here be given.
_Acetic amyl ether_ or _amyl acetate_, C_{5}H_{11}O.C_{2}H_{3}O, is
prepared by mixing 1 part of amyl alcohol with 1 part of concentrated
sulphuric acid, and distilling the mixture with 2 parts of potassium
acetate. The distillate is washed with water, to which some carbonate
of soda has been added, and then rectified over magnesia. It forms a
colorless liquid of an agreeable fruity odor. It boils, according to
Kopp, at 280° F. and, at 59° F., its specific gravity is 0.8692.
For use in perfumery, the ether is best prepared, according to
Fehling's directions, by heating for some time at a temperature of 212°
F. 1 part of glacial acetic acid with ½ part of sulphuric acid and
one part of amyl alcohol. By then adding water the ether is separated.
By this process distillation is avoided.
_Acetic ethyl ether_ or _ethyl acetate_, C_{2}H_{3}O.O.C_{2}H_{5}.
Acetic ether is formed by the decomposition of sodium acetate by ethyl
sulphuric acid:--
SO_{2} {OC_{2}H_{5} + C_{2}H_{3}O.ONa =
{OH
└----┬-----┘ └------┬------┘
Ethyl sulphuric Sodium acetate.
acid.
SO_{2} {ONa + C_{2}H_{3}O.OC_{2}H_{5}
{OH
└--┬--┘ └---------┬----------┘
Acid sodium Acetic ether.
sulphate.
One molecule of sulphuric acid or 98 parts is mixed with one molecule
of alcohol or 46 parts, or with 1 molecule of alcohol of 90 per
cent. which contains 85.75 per cent. of absolute alcohol, hence
with 53.6 parts of alcohol, and distilled with 1 molecule or 82
parts of anhydrous sodium acetate. Since commercial sulphuric acid
always contains 5 or 6 per cent. of water, this has to be taken into
consideration, and 105 to 106 parts of it have to be used in order
to decompose the entire quantity of sodium acetate. The crude sodium
acetate found in commerce may be used. It is nearly white and at the
utmost contaminated by traces of sulphuric acid and chlorine, which in
this case are not injurious. The crystallized salt is heated in an iron
kettle whereby it melts in its water of crystallization. With constant
stirring the water is then completely evaporated until an entirely
dry mass of salt remains behind. The latter may be quite strongly
heated without fear of destroying the acetic acid. The dried salt is
immediately powdered, passed through a medium fine sieve and kept for
use in well-closed vessels.
On a large scale the distillation of the ether may be effected in an
iron kettle, which is provided with a well-fitting lid and connected
by a copper head with a cooling apparatus--a worm lying in cold water.
Bring into the kettle the required quantity of concentrated sulphuric
acid, add, with vigorous stirring, the alcohol and allow the mixture to
rest for 24 hours. Then throw the dry sodium acetate into the mixture,
mix it thoroughly, by stirring, with the ethyl sulphuric acid, and,
after luting all the joints of the apparatus, heat at first moderately.
Distillation proceeds quietly and uniformly, the fire being regulated
according to how the ether runs off from the worm. Such uniform
distillation is, however, only attained by the use of the sodium
acetate in the form of powder, and thoroughly mixing it with the acid.
If large pieces of the salt are present or the powdered salt balls
together, the formation of ether sometimes takes place so suddenly
that the vapors cannot condense in the cooling apparatus, but escape
violently, or if they cannot escape rapidly from the condenser, may
even burst the apparatus. The reason for this is that the larger pieces
float in the superheated acid without being saturated by it, and, when
they suddenly collapse, form a mass of ether-vapors.
Distillation is continued until that which at last passes over is not
inflammable. With the above-mentioned proportions 88 parts of acetic
ether are formed, but as some water always passes over, distillation
need not be interrupted until the receiver contains at least 90 parts
of crude ether.
The crude ether always contains more or less water, some alcohol,
and a small quantity of free acetic acid. With the above-mentioned
proportions, the content of alcohol can, however, be only very small.
To neutralize the acetic acid, add some burnt magnesia or shake with
carbonate of soda solution until the acid reaction disappears. For the
absorption of the water and alcohol, add as much sharply dried (not
fused) calcium chloride as the fluid will dissolve, and then let it
stand with an excess of the salt for one day. The calcium chloride
combines with the water and alcohol and separates as a heavy layer
beneath the ether. The latter is decanted off and brought into a
rectifying vessel--a copper still, heated by steam, and provided with a
cooling pipe. The ether is distilled off at a moderate heat, the last
portion, about 1/10, being caught in a special receiver, to be again
rectified at the next operation.
According to Grossschopf, 40 lbs. of pulverized anhydrous sodium
acetate, together with a cooled mixture of 46 lbs. of concentrated
sulphuric acid and 37 lbs. of 95 per cent. alcohol, free from fusel
oil, are distilled in a copper still heated by steam. Distillation
is continued with constant stirring by means of an apparatus in the
still, until no more fluid smelling and tasting of acetic ether passes
over. The crude distillate, amounting to 55 or 56 lbs., is brought into
bottles which are filled ⅔ full. The bottles are then filled up with
water and potassium carbonate is added until the fluid, after shaking,
shows no acid reaction. The aqueous fluid beneath the ether is then
drawn off by means of a siphon, and the ether several times washed by
shaking with water and allowing to settle. Since the wash-water absorbs
a quite considerable quantity of ether, it is collected and subjected
to rectification, whereby an alcoholic acetic ether is obtained. The
ether, being freed from acetic acid and alcohol by neutralization and
washing, is brought in contact with fused calcium chloride to free it
from water, and finally rectified over magnesia. In this manner 36 to
37 lbs. of pure acetic ether are obtained.
Acetic ether is a clear, colorless fluid of a pleasant, etheral odor.
It boils at 170.6° F., and at 59° F. its specific gravity is 0.9068.
Pure acetic ether dissolves in 11 to 12 parts of water; a content of
alcohol or the addition of water increases its solubility. Hence, its
solubility in water is a criterion of its purity.
_Benzoic ether_ or _ethyl benzoate_, C_{7}H_{5}O.OC_{2}H_{5}, is most
readily prepared by mixing 4 parts of alcohol, 2 parts of crystallized
benzoic acid, and 1 part fuming hydrochloric acid, and for some time
heating the mixture in a flask. The benzoic acid is thereby gradually
and completely converted into ether. The fluid is mixed with water,
whereby the ether is completely separated. It is several times washed
with carbonate of soda solution, and, for the purpose of withdrawing
the last trace of free acid, distilled over lead oxide. It forms a
colorless oil of an aromatic odor, specific gravity 1.0502, and boils
at 412° F. In cold water it is insoluble. However, like all varieties
of ether, it dissolves readily in alcohol and ether.
_Butyric ethyl ether_ or _ethyl butyrate_, C_{4}H_{7}O.OC_{2}H_{5}. The
preparation of this ether must be preceded by that of butyric acid.
The latter is obtained, according to Bensch, by dissolving 6 lbs. of
cane sugar and 8 drachms of tartaric acid in 13 quarts of hot water,
allowing the liquid to stand a few days and then adding 7 ozs. of old
rotten cheese, which has been stirred up in 4 quarts of skimmed sour
milk and 3 lbs. of finely pulverized chalk. The mixture must be kept
at a uniform temperature of from 86° to 95° F. for some weeks, from
time to time mixing it by stirring, and replacing the water lost by
evaporation.
By the action of a ferment the sugar is first converted into lactic
acid. In 10 to 12 days the entire mass congeals to a paste of calcium
lactate. By now allowing fermentation to proceed without interruption,
it gradually enters another stage; gas bubbles consisting of carbonic
acid and hydrogen rise up, until in the course of 5 or 6 weeks the
process is finished. This is recognized by the fluid becoming quiet,
no more gas being evolved. The fluid then contains a solution of
calcium lactate, which is converted into the corresponding sodium salt
by the addition of 8 lbs. of crystallized soda. It is then filtered
and concentrated by evaporation to 5 quarts. By adding 5½ lbs. of
sulphuric acid, diluted with an equal volume of water, butyric acid is
separated as a dark-colored oily mass.
The crude butyric acid thus obtained and freed from water by shaking
with calcium chloride, is a mixture of acetic, butyric, and capric
acids, but does not contain propionic and valerianic acids. To obtain
from it pure butyric acid, fractional distillation is required. For
manufacturing on a large scale, a copper distilling apparatus with
silver head and silver cooling pipe is used, the bulb of a thermometer
being placed in the head. In the first rectification, the receiver
is changed after the thermometer has risen to 311° F.; the portion
passing over between 311° and 329° F. is caught up by itself, and
the receiver being again changed, distillation is continued until
finished. The first distillate contains mostly acetic acid, besides
a small quantity of butyric acid, the second the greater portion of
the butyric acid besides a little acetic and capric acids, while the
third consists chiefly of capric acid. For preparing butyric ether for
technical purposes, the fraction passing over between 311° and 329°
F. is sufficiently pure. To obtain chemically pure butyric acid, the
rectification of the portion passing over between 311° and 329° F. is
in the same manner repeated, until finally a product with a constant
boiling point at 324.2° F. is obtained.
Butyric acid fermentation proceeds more rapidly by using, instead of
rotten cheese, putrefying meat, and in place of sugar, starch paste
or mashed boiled potatoes, 1 part of meat to 4 parts of starch or a
corresponding quantity of potatoes being employed. The same products
are formed as in the preceding process, but much more rapidly,
fermentation being finished, according to Schubert, in 5 to 6 days.
Butyric acid, C_{4}H_{7}O.OH, or C_{3}H_{7}COOH, is a liquid of a very
sour taste and odor, and at an intense cold congeals to a crystalline
mass which melts at 32° F. In a pure state it boils at 324.2° F. It is
soluble in water, but separates again if soluble salts are added to
this solution. Its specific gravity, after being completely freed from
water, is 0.974.
Besides the normal butyric acid, there is known another one called
_isobutyric' acid_ or _dimethyl acetic acid_. It is distinguished from
the normal acid by being less soluble in water and by its boiling
point, which lies at 309.2° F. It occurs in St. John's bread or carob,
in the volatile oil from _Arnica montana_ and in croton oil.
_Butyric ether_ is formed by mixing 2 parts of butyric acid with 2
parts of alcohol and 1 part of sulphuric acid. The fluid is heated to
176° F., and, after being for several hours kept at that temperature,
is poured into cold water, whereby the ether separates as an oily
fluid. It is then separated from the aqueous solution, washed with
water to which some chalk has been added for the neutralization of the
free acid, and finally the water is withdrawn from the ether by, for
several days, leaving it in contact with calcium chloride. To obtain
it entirely pure, it is only necessary to distil it once. It forms a
clear, very mobile fluid of a pine-apple odor, and a specific gravity
of 0.900. It boils at 249.8° F.
Commercial butyric ether, large quantities of which are used for the
preparation of the so-called _pine-apple ether_ or _essence_, is seldom
pure, it being generally obtained from simply rectified butyric acid.
According to another method, which is, however, not as profitable,
it is obtained by distilling butter-soap with alcohol and sulphuric
acid. For this purpose, bring 20 pounds of butter-soap, cut up in
small pieces, into a distilling apparatus, pour over it 10 pounds of
90 per cent. alcohol and heat moderately until the soap is dissolved.
Since a portion of the alcohol evaporates thereby, add 10 pounds more
of alcohol and then 20 pounds of sulphuric acid. On further heating,
a fluid of a very agreeable odor distils over, which is an alcoholic
solution of the ethers of the volatile acids found in butter. Towards
the end of the operation, in consequence of the further progress of
decomposition, a development of sulphurous acid generally takes place.
This is removed from the distillate by allowing it to remain for
several days in contact with finely-pulverized pyrolusite (peroxide
of manganese) and rectifying over burnt magnesia. In the first
distillation, the heavy volatile acids of the butter remain behind;
they are freed from the excess of sulphuric acid and the sulphate of
sodium or potassium by washing with hot water, and can be utilized in
the manufacture of soap.
The butyric ether obtained from butter-soap is far from being pure
butyric ether, it containing, besides it, a mixture of various kinds of
ether derived from the volatile acids--caproic, capric, and caprylic
acids. However, these varieties of ether possess similar properties
to that of butyric acid; in alcoholic solutions their taste and odor
are nearly alike, and hence can be employed in this mixture for the
preparation of essences of an agreeable odor and taste.
A suitable material for the preparation of butyric ether is also the
St. John's bread or carob, the pods of _Silequa dulcis_. Redtenbacher
established in them the occurrence of about 2 per cent. butyric acid,
which Gruenzweig later on proved to be isobutyric acid. Besides butyric
acid and other volatile acids, St. John's bread contains about 40 per
cent. of fermentable varieties of sugar, which can be utilized after
their conversion to butyric acid. For this purpose Stinde has proposed
the following process: Convert the pods together with the seeds to a
coarse powder; bring 100 lbs. of this powder into a capacious barrel
placed in a warm place, and pour sufficient water of 82.5° F. over it,
to form a thin paste; after 4 to 5 days add 24 lbs. of whiting and
await fermentation. The paste, which gradually becomes thicker, is from
time to time stirred, and, if necessary, a small quantity of lukewarm
water added. In summer fermentation is finished in six weeks, after
which the preparation of the ether is proceeded with.
For this purpose bring the paste into a still provided with a steam
jacket; the evening before mix 36 lbs. of concentrated sulphuric acid
with 60 lbs. of alcohol of 95 per cent., and add the mixture to the
paste in the still; then lute the joints of the distilling apparatus,
and quickly introduce steam. Distillation soon commences, and, when
once introduced, is continued with a moderate admission of steam.
The first pound of the distillate is caught by itself, and, after
changing the receiver, distillation is continued until but little
passes over, even with an increased admission of steam. Thus
an abundant yield of alcoholic butyric ether is obtained. When
distillation is finished 20 lbs. more of alcohol may be brought into
the still; the distillate obtained thereby being still rich in butyric
ether.
The St. John's bread used should be of the best quality, free from
worms and mould, as otherwise the ether would not possess the pure,
agreeable odor characteristic of butyric ether.
_Formic ethyl ether_, or _ethyl formate_, CHO.OC_{2}H_{5}.--This ether
is also much manufactured for the preparation of the so-called essences
which are employed for the purpose of imitating the odor of plants,
fruits, etc. It is formed by the action of formic acid upon alcohol, or
by bringing ethyl sulphuric acid, or a mixture of alcohol and sulphuric
acid, in contact with formates, or finally by bringing formic acid at
the moment of its formation in contact with alcohol.
The most simple process is that recommended by Lorin:--
Into a capacious distilling apparatus connected with the cooling pipe,
so that the distillate constantly flows back, bring 1 part, by weight,
of glycerin of the consistency of syrup, add ¼ of its weight of
crystallized oxalic acid and the same quantity of alcohol of 90 to 95
per cent. With moderate heating a vigorous development of gas soon
takes place. The oxalic acid in contact with the glycerin splits into
formic acid and carbonic acid, according to the following equation:--
{COOH = CHO.OH + CO_{2}.
{COOH
└--┬--┘ └----┬----┘ └--┬--┘
Oxalic acid. Formic acid. Carbonic acid.
The glycerine does not undergo alteration thereby. The nascent formic
acid converts the alcohol present into formic ether, water being
separated. When, after continued heating, the development of carbonic
acid abates, add the same quantities of oxalic acid and alcohol to
the contents of the still, heat again until but little carbonic acid
is evolved, and then add, twice in succession, the same quantities of
oxalic acid and alcohol as before, until finally as much oxalic acid is
consumed as glycerin has been employed. When the evolution of carbonic
acid ceases, the receiver is reversed and the ether distilled off. The
glycerin remaining behind is again concentrated to the consistency of
syrup, and may be re-used.
The distillate is freed from free acid by the addition of magnesia, and
the alcohol and water are separated by shaking with calcium chloride,
after which the pure ether is obtained by rectification.
Formic ether is colorless, thinly-fluid, of a pleasant smell, specific
gravity 0.945, boiling point 130° F., soluble in cold water, and
miscible in every proportion with alcohol and ether.
_Nitrous ether_, or _ethyl nitrite_, C_{2}H_{5}.ONO.--In a pure state
this ether is best prepared according to the method given by E. Kopp.
It consists in bringing equal volumes of alcohol and ordinary nitric
acid together with copper filings into a distilling apparatus, which
is so arranged that the vapors first pass through a flask filled with
water of 77° F., then through a calcium chloride tube, and are finally
condensed in a receiver surrounded by snow and common salt. The nitric
acid is first decomposed by the copper, nitrous acid being thereby
developed, which is so transposed that its radicle NO occupies the
position of the typical hydrogen in the alcohol, while the rest of the
acid forms water with the hydrogen of the alcohol. By the reaction such
a quantity of heat is liberated that the process requires assistance by
external heating only towards the end of the operation. In the receiver
is then a pale yellow fluid having the taste and odor of apples and, at
59° F., a specific gravity of 0.947. According to Liebig, the boiling
point of nitrous ether lies at 61.5° F.; hence it can be condensed only
by careful cooling, and has to be kept in glass tubes fused together.
In water it is but sparingly soluble, but readily so in alcohol. By the
addition of water it is separated from the alcoholic solution.
Mohr has modified Kopp's method as follows: Mix alcohol of 0.833
specific gravity, water, and nitric acid of 1.200 specific gravity,
each 24 parts and add 4 parts of copper filings. Of this mixture draw
off 24 parts of distillate, mix the latter with litmus tincture and
neutralize the free acid by adding, drop by drop, solution of caustic
potash or soda until the litmus tincture becomes blue. Rectify the
distillate and catch of it 8 parts. Compound the latter with 16 parts
alcohol of 0.833 specific gravity, whereby the product is made equal to
the quantity of alcohol originally used. The product is kept in glasses
holding from 2 to 3 ozs. each. This alcoholic nitrous ether is of a
yellow color, very strong and has a pure odor.
In England and America, nitrous ether is much used for aromatizing
whiskies and for other purposes. According to Stinde[9] it is prepared
on a large scale as follows:--
A stone-ware flask of at least 120 lbs. capacity, such as is used for
the preparation of chlorine, is so placed upon a tripod in a sheet-iron
cylinder that the neck projects over the edge of the cylinder. The
space between the flask and the walls of the cylinder is completely
filled with mats or coarse pack-cloth. A steam-pipe enters the lower
part of the cylinder, while a cock placed on the bottom of the cylinder
serves for discharging the condensed water. The cylinder is closed by
a sheet-iron cover provided in the centre with a hole through which
passes the neck of the flask. The flask is filled with 60 lbs of 90 per
cent. alcohol free from fusel oil, to which, in small portions, 15 lbs.
of crude nitric acid of 36° Bé. are added.
[9] Dingler's Polyt. Journ., 184, 367.
The neck of the flask is provided with an exactly-fitting tube of pure
tin. The tube is bent twice at a right angle, and one end is provided
with an annular piece to prevent it from slipping too far into the
interior of the flask. The joints between the tube and the neck of the
flask are luted with a stiff paste of flaxseed meal, a wet strip of
linen being, for greater security, wrapped over the cement. The other
end of the tin-tube, which here occupies the place of a still-head,
is in the same manner connected with a long tin-worm lying in a large
cooling vat.
Everything being prepared, but little steam is at first introduced
into the iron cylinder in order to slowly warm the apparatus. When
this is done the admission of steam is gradually increased. The mats
or pack-cloth placed between the walls of the cylinder and the flask
prevent the latter from bursting, which otherwise might readily happen.
Distillation commences in about ten minutes. The admission of steam
is then moderated, care being had that the ether passes over in an
uninterrupted stream of the thickness of a goose-quill.
When, with the admission of the same amount of steam, the distillate
commences to run drop by drop, the steam-cock is closed and the
operation interrupted, this being the case in about six to seven hours.
The next day the flask--without removing the residue--is charged in
the same manner. However, the third day only 30 pounds of alcohol are
poured in.
The combined distillates come into a copper still with double walls,
between which steam can be admitted, and are neutralized with dry
calcium hydrate. The cooling pipe connected with the still consists of
tin, and is provided with a beak dipping into a flask filled half-full
with 4 pounds of alcohol. A slight current of steam suffices for
distillation. The first distillate is dark yellow, and contains large
quantities of aldehyde. Notwithstanding careful cooling, the vapors can
be but incompletely condensed, and their inhalation has to be carefully
avoided, they producing stupor and headache as well as inflammation of
the eyes. When the distillate is colorless and shows no reaction with
litmus paper, the receiver is removed and replaced by a large glass
balloon in which the entire distillate is collected. Distillation must
be quickly finished, as otherwise colored ether is obtained.
_Valerianic amyl ether_ or _amyl valerate_, C_{5}H_{11}O.C_{5}H_{9}O.
This ether is formed by treating amyl alcohol with chromic acid.
However, besides the ether a large quantity of valerianic acid is also
formed, which has to be converted by itself into ether.
To prepare the ether bring 5½ parts of powdered potassium dichromate
together with 5 parts of water into a distilling apparatus and very
gradually add a mixture of 1 part amyl alcohol and 5 parts concentrated
sulphuric acid. The fluid becomes so strongly heated that it almost
boils. When reaction is finished, heat and distil off the rest. The
distillate consists of two layers; the lower one being an aqueous
solution of valerianic acid and the upper one a mixture of valerianic
acid and amyl valerate. To separate both, add concentrated carbonate of
soda solution until all the free acid is neutralized. The oily liquid
separating thereby is the ether. It is separated from the valerianate
of sodium, the latter evaporated to a small volume, and, after cooling,
sufficient sulphuric acid to fix the entire quantity of the soda is
added. The valerianic acid is thereby separated, and floats upon the
solution of the sodium sulphate. It is separated from the latter, and
1¼ parts of it are added to a mixture of ¾ part of amyl alcohol and 1
part sulphuric acid and heated to 212° F. After the addition of water,
the apple-ether separates and only requires washing with water and some
sodium carbonate to yield a pure product.
The separation of the valerianic acid can, however, be readily avoided.
Evaporate the neutral solution of the valerianate of soda to dryness in
the water-bath, weigh off 1 molecule, or 124 parts, and gently heat it
with a mixture of 1 molecule or 98 parts of sulphuric acid (on account
of the content of water in the commercial acid, 105 parts of it will
have to be taken) and 1 molecule or 88 parts of amyl alcohol.
The ether thus obtained is a fluid, which, in a concentrated state,
does not possess an agreeable odor, but when mixed with 10 parts of
alcohol imparts to the latter an odor resembling that of apples. It
boils at from 370° to 374° F., and at 64° F. has a specific gravity of
0.8793.
_Valerianic ethyl ether_ closely resembles the amyl ether, and, like
it, is prepared from valerianate of sodium, ordinary alcohol, and
sulphuric acid.
_Apple ether_ essentially consists of valeric amyl ether, of which 1
part is dissolved in 6 to 10 parts of strong alcohol.
_Apricot ether_ is butyric ether with some amyl alcohol.
_Cherry ether_ is acetic ether with benzoic ether.
_Pear ether_ contains acetic amyl ether.
_Pineapple ether_ is butyric ether.
_Strawberry ether_ is acetic ether with acetic amyl ether and butyric
ether.
The ethers are dissolved in various proportions in alcohol, according
to the intensity of the odor which it is desired to obtain. The
aroma of most of them is generally increased by a slight addition of
chloroform.
For the preparation of different fruit essences Kletzinsky[10] gives
the following directions. The figures indicate additions in cubic
centimeters to 1 liter of rectified alcohol of 90 per cent.:--
[10] Dingler's Polyt. Journ., 180, 77.
_Apple essence._--Chloroform 10, nitrous ether 10, aldehyde 20, acetic
ether 10, valeric amyl ether 100, oxalic acid[11] 10, glycerin 40.
_Apricot essence._--Chloroform 10, butyric ether 100, valeric ether
50, peach oil 10, amyl alcohol 20, butyric amyl ether 10, tartaric
acid[11] 10, glycerin 40.
_Cherry essence._--Acetic ether 50, benzoic ether 50, peach oil 10,
benzoic acid[11] 10, glycerin 30.
_Currant essence._--Aldehyde 10, acetic ether 50, benzoic ether 10,
grape-seed oil 10, tartaric acid[11] 50, succinic acid[11] 10, benzoic
acid[11] 10.
_Grape essence._--Chloroform 20, aldehyde 20, formic ether 20,
grape-seed oil 100, wintergreen oil 10, tartaric acid[11] 50, succinic
acid[11] 30, glycerin 100.
_Lemon essence._--Chloroform 10, nitrous ether 10, aldehyde 20, acetic
ether 100, oil of lemons 100, tartaric acid[11] 100, succinic acid[11]
10, glycerin 50.
_Melon essence._--Aldehyde 20, formic ether 10, butyric ether 40,
valeric ether 50, glycerin 30.
_Orange essence._--Chloroform 20, aldehyde 20, acetic ether 50,
formic ether 10, butyric ether 10, benzoic ether 10, wintergreen oil
10, acetic amyl ether 10, orange-peel oil 100, tartaric acid[11] 10,
glycerin 100.
[11] The figures for free acids refer to cubic centimeters of cold,
saturated, alcoholic solutions.
_Peach essence._--Aldehyde 20, acetic ether 50, formic ether 50,
butyric ether 50, valeric ether 50, peach oil 50, amyl alcohol 20,
glycerin 50.
_Pear essence._--Acetic ether 50, acetic amyl ether 100, glycerin 100.
_Pineapple essence._--Chloroform 10, aldehyde 10, butyric ethyl ether
50, butyric amyl ether 100, glycerin 30.
_Plum essence._--Aldehyde 50, acetic ether 50, formic ether 10, butyric
ether 20, peach oil 40, glycerin 80.
_Raspberry essence._--Nitrous ether 10, aldehyde 10, acetic ether 50,
formic ether 10, butyric ether 10, benzoic ether 10, grape-seed oil
10, wintergreen oil 10, acetic amyl ether 10, butyric amyl ether 10,
tartaric acid[11] 50, succinic acid[11] 10, glycerin 40.
[11] The figures for free acids refer to cubic centimeters of cold,
saturated, alcoholic solutions.
_Strawberry essence._--Nitrous ether 10, acetic ether 50, formic ether
10, butyric ether 50, wintergreen oil 10, acetic amyl ether 30, butyric
amyl ether 20, glycerin 20.
CHAPTER VIII.
ALCOHOLIC PERFUMES.
The alcoholic perfumes, also called "_Extraits d'Odeurs_," are divided
into flower-odors, "_Extraits aux fleurs_," and into compound odors,
"_Bouquets_." The extracts of French flower pomades form the foundation
of all _Extraits d'Odeurs_, all other additions serving the purpose of
rendering these odors more pronounced and durable. Hence the art of the
perfumer consist in attaining this object as perfectly as possible by
the correct composition of the perfume-materials at his disposal. If,
for instance, the flower-odor _jasmine_ is to be prepared, it would not
be sufficient to simply use the alcoholic extract of jasmine-pomade for
the purpose, since the odor of jasmine would soon volatilize in the
air or upon the handkerchief, if the perfumer did not understand how
to prevent it. To prevent the rapid volatilization of the scent, to
retain it or to fix it, extracts of various perfume-materials, known as
tinctures or extracts are used.
The method of preparing the flower-pomades in France has already been
described on p. 58 _et seq._ It need here only be added that, according
to their quality, these pomades are designated by different numbers
by the French manufacturers. There are three qualities, which by some
manufacturers are designated as No. 6, No. 18, and No. 30; and by
others as No. 12, No. 24 and No. 36, so that No. 6 and No. 12, No. 18
and No. 24, as well as No. 30 and 36 correspond to each other. Pomades
No. 6 or No. 12 are not suitable for the preparation of extracts, they
containing but little actual extract of flowers, and are generally
mixtures touched up with volatile oils. They are almost exclusively
used for hair pomades, for which they are well adapted. No. 18 or No.
24 is the quality generally employed by the perfumer for alcoholic
extracts. No. 30 or No. 36 is the strongest, and, hence, most expensive
flower-pomade, and is used only by a few perfumers who have customers
for the finest qualities of _Extraits d'Odeurs_.
When freshly prepared, the above-mentioned flower pomades do not
possess the fine odor of the respective flowers, the full aroma being
developed only after about six months. The tin-canisters containing
them should be provided with well-fitting lids and kept in a cool, dry
cellar. Thus stored, flower-pomade keeps for about five years, with the
exception of jasmine and tuberose, which keep only for about two years.
In order to show how the extraction of flower-pomades is effected,
we will take, as an example, 2 lbs. of French flower-pomade No. 18
and 3½ quarts of best alcohol.[14] This proportion yields a good and
sufficiently strong extract for the preparation of _Extraits d'Odeurs_.
It must, of course, be suited to the size of the extracting apparatus,
8 lbs. of flower-pomade and 14 quarts of alcohol being, for instance,
taken, though that depends on the quantity of the respective extract
required by the perfumer. It is, however, best that the apparatus
should be as completely filled as possible so that it contains but
little air.
[14] By "best alcohol" is understood rectified alcohol of 95 to 97 per
cent.
The gaining of alcoholic extracts from flower-pomades is best effected
in a special apparatus, one of the simplest kind for the purpose being
shown at Fig. 25.
[Illustration: FIG. 25.]
It consists of two cylinders, _A_ and _A_{1}_ of stout sheet-iron
provided with well-fitting lids. Through the centre of each lid passes
a vertical iron shaft _a_ and _a_{1}_ which carries in the interior
of the apparatus several horizontal arms _b_, _b_{1}_, _b_{2}_. These
vertical shafts can be rapidly revolved by the horizontal shaft _c_.
Before bringing the flower-pomade into the apparatus, it is melted in
the water-bath at a temperature, which, under no conditions, should
exceed 88.25° F. The alcohol is also heated to 88.25° F. and added to
the melted pomade in the apparatus. The arms with which the vertical
shaft is provided, keep the mass in the apparatus in constant motion
and prevent the pomade from settling on the bottom. The apparatus is
arranged to be driven either by hand or steam, a fly-wheel instead of a
pulley, being in the first case provided at _g_.
Where the manufacturer has steam-power at his disposal, the apparatus
may be connected with the transmission and allowed to run for 48 to 60
hours during working time. After the expiration of this time, proceed
to strain off the finished extract (No. 1) as follows: Over a clean tin
vessel stretch a close, white linen cloth, and pour the entire contents
of the apparatus upon the latter; the liquid portion runs through the
cloth into the vessel, while the pomade remains behind upon the cloth.
Finally, the cloth is thoroughly wrung out in order to obtain as much
alcoholic extract from the pomade as possible. Bring the extract, No.
1, thus obtained into a glass flask, allow it to stand in a cool cellar
for about 48 hours, and then filter it through paper into another glass
bottle. This filtering through paper is necessary, even if the extract
should appear clear and pure, as, in straining, not only do small
particles of fat pass through the cloth, but are also dissolved in the
extract. By quietly standing in a cool cellar these particles of fat
are separated and appear as white flakes on the bottom and sides of the
flask. At a higher temperature, these flakes melt and appear as drops
of oil on the bottom of the flask. If filtering were omitted, these
particles of fat would be transferred to the extracts and thus cause
stains upon handkerchiefs, clothing, etc. If the manufacturer has not a
cool cellar at his disposal, the fatty particles are readily separated
by placing the flasks containing the extract upon ice, and filtering
immediately after separation is complete. The fat then remains upon the
filter.
The pomade remaining upon the straining cloth is, without being
previously melted, returned to the apparatus, and, after adding the
same quantity of alcohol (3½ quarts to every 2 lbs. of pomade), the
mixture is again worked as previously described. The straining off and
filtering of extract No. 2 is effected in precisely the same manner as
extract No. 1.
The pomade upon the cloth is now brought for the third time into the
apparatus and, after adding 3½ quarts of alcohol for every 2 lbs. of
pomade, subjected to the same treatment as for extracts Nos. 1 and 2.
After thoroughly wringing out the cloth containing the pomade, the
latter is brought into a clean tin vessel and entirely melted upon
the water-bath. The vessel containing the melted pomade is placed in
a cool cellar and, if after complete cooling, a liquid appears upon
the surface, it is added to the flask containing extract No. 3. This
extract, No. 3, is used in place of alcohol when preparing, the next
time, extract No. 1 from the same kind of pomade. In this manner, an
extract No. 1 of still greater strength is obtained, and by treating
the pomade three times with alcohol, it is more completely exhausted.
The exhausted pomade can, in conjunction with fresh fat, be used for
ordinary hair pomades.
Although the extraction of pomades is somewhat laborious and requires
great care, it nevertheless pays the perfumer.
[Illustration: FIG. 26.]
Beyer frères, of Paris, have essentially improved the extracting
apparatus previously described, the improvement being shown in Fig. 26.
The cylinders _A_ and _A_{1}_ are of copper tinned inside; the lids
close air-tight; above the cocks _f_ and _f_{1}_ a perforated piece of
tin is placed in the interior of the cylinders; upon this piece of tin
a disk of felt may be placed, and thus the extract be drawn off clear.
In order to reduce the pomade to a finely divided state, and thus bring
it in contact with the alcohol, it is passed through a vermicelli
press, _h_, placed upon the cylinder _A_{1}_. The pomade passes, in
the form of fine vermicelli, through a sieve in the lower portion of
the press into the alcohol contained in the cylinders. The press can
be transferred from one extracting vessel to the other. The shafts _a_
and _a_{1}_ also have several horizontal arms like those shown in Fig.
25. Through the contrivances _d_ and _d_{1}_, sitting upon the shaft
_c_, the shafts _a_ and _a_{1}_, receive a revolving as well as an
up-and-down motion, so that a complete mixture of pomade and alcohol is
effected. By this arrangement the pomade completely yields its perfume
to the alcohol in one day, and independent of the quicker work, it
has the further advantage that the extracts are of better quality in
consequence of not remaining for so long a time in contact with the fat.
TINCTURES AND EXTRACTS. In the following pages receipts for the
preparation of the principal tinctures and extracts used in the
preparation of _Extraits_, as well as in other branches of perfumery,
fumigating pastils and powders, dentifrices, mouth-waters, and
cosmetics, will be given. The tinctures are prepared from the
resins and balsams previously mentioned, as well as from the
perfume-substances derived from the animal kingdom. Besides these
there are employed for the purpose several spices, leaves, roots, and
seeds--such as musk-seeds, angelica root, orris root, patchouli leaves,
musk-root or sumbul-root, tonka beans, vanilla, vitivert root, etc.
Most of these substances, if not already found in commerce in the form
of a powder, are, before extraction, pulverized, or at least comminuted
as much as possible. For a better view the treatment of each substance
is given with the respective receipt. The infusions should be stored in
a moderately warm room, and thoroughly shaken several times every day.
When extraction is finished the product is filtered through paper and
is then called _tincture_ or _extract_.
The substances to be used for tinctures should be fresh and genuine,
and the alcohol free from fusel oil, since a perfect tincture can only
be obtained under these conditions. For the preparation of tinctures
Beyer frères have constructed very suitable apparatuses (Figs. 27 and
28). By the vigorous and uninterrupted agitation produced by means of
such an apparatus extraction is effected much more rapidly and more
completely than by treating the substances to be extracted in ordinary
bottles and by shaking with the hand.
[Illustration: FIG. 27.]
The apparatus (Fig. 27) is provided with two boxes for the reception
of bottles filled with the substances to be extracted and alcohol.
In the accompanying illustration one box is charged with two glass
bottles and the other with a copper flask. However, Beyer frères also
construct apparatuses which can, at one time, be charged with 6, 8,
or 10 glass bottles, so that 6, 8, or 10 different tinctures can be
prepared at one operation.
[Illustration: FIG. 28.]
The apparatus (Fig. 28) consists of a round table provided with
cavities covered with leather, in which rest bottles of a special
shape. The bottles fit exactly in the cavities. The stoppers, with
which the bottles are closed, rest against a screw of large diameter
placed in the centre of the apparatus. Against this screw the bottles
are firmly pressed by means of clamps and screws. The bottles being
filled with the substances to be extracted, the table is set in motion,
moving alternately from left to right and from right to left.
It is advisable to have always a sufficient supply of tinctures on
hand, since their aroma improves by age.
The receipts given in the following pages have been practically tested
and can be recommended as perfectly reliable.
_Musk tincture._--Tonkin musk 11 drachms, rose water 8 ozs., best
quality of alcohol 2 quarts.
Carefully empty the musk sac into a glass flask, add the rose water and
let the flask stand for about 10 days, shaking frequently. Then add the
alcohol and let the whole stand for several weeks, shaking frequently.
Cut up the empty musk sacs into as small pieces as possible, and,
in another bottle, treat them in the same manner as their contents;
distilled water, may, however, be used instead of rose water. The
object of the water is to soften the musk, which swells up, so that the
alcohol can better penetrate into the cellular tissue and absorb the
aroma.
The extract from the empty musk sacs is used for cheaper products, or
mixed with the extract from the contents of the sacs, according to
whether a more or less fine quality of tincture is to be obtained. A
still higher yield might, perhaps, be obtained by the use of a machine
for comminuting the musk, which grinds the sac to atoms, whereby the
cellular tissue is still more completely disintegrated than by cutting
up.
_Civet tincture._--Civet 5½ drachms, best quality of alcohol 3 pints.
Civet in its natural state being, with difficulty, soluble in alcohol,
triturate it in a mortar to a pulverulent mass together with some dry
substance, for instance, whiting or exhausted orris-root powder. The
mixture is then brought into a glass flask, the alcohol added, and the
whole frequently shaken.
_Ambergris tincture._--Ambergris 5½ drachms, alcohol of the best
quality 1 quart.
Ambergris dissolving readily in alcohol, pulverizing is not required,
but if it is done, great care should be exercised to prevent loss of
this expensive substance. Ambergris is not so much distinguished by its
aroma as by its indestructibility, which renders it especially suitable
for fixing odors.
_Castor tincture._--Castor 3½ ozs., best quality of alcohol 3 pints.
Comminute the castor as much as possible, bring it into a glass flask
and add the alcohol.
Perfume-substances resembling musk having in the last few years
increased to an extraordinary degree, the use of castor has been almost
entirely abandoned on account of its disagreeable odor. The tincture
can only be employed, when very old, for cheap perfumes.
_Benzoin tincture._--Benzoin (Siam) 2 lbs., best quality of alcohol 3
quarts.
Convert the benzoin into a coarse powder, bring it into a flask, add
the alcohol and shake thoroughly. Solution takes place in 10 to 12 days.
Siam benzoin is the finest and most expensive and is indispensable for
_Extraits d'Odeurs_. For cheaper products of perfumery, Sumatra benzoin
answers very well.
_Peru-balsam tincture._--Peru balsam 8 ozs., best quality of alcohol 5
quarts.
_Tolu-balsam tincture._--Tolu balsam 3 lbs., best quality of alcohol 5
quarts.
Bring the alcohol into a bottle. Tolu balsam cannot be reduced to a
powder, hence it is necessary to keep it right cool, whereby it becomes
brittle so that it can be cut up with a sharp instrument and a hammer.
The pieces detached are rapidly brought into the alcohol, solution
taking place in about 14 days. If the alcohol were added to the tolu
balsam, the latter would ball together, rendering solution very
difficult. Frequent vigorous shaking is necessary.
_Olibanum tincture._--Olibanum 2 lbs., best quality of alcohol 4 quarts.
Reduce the olibanum to as fine a powder as possible, bring it into a
flask, add the alcohol and shake frequently.
_Opopanax tincture._--Opopanax 2 lbs., best quality of alcohol 4 quarts.
Reduce the opopanax to a coarse powder, bring it into a bottle, add the
alcohol and shake frequently.
_Storax tincture._--_Storax liquidus_ 4 lbs., alcohol of best quality 5
quarts.
Bring the alcohol first into the flask. Then place the pot containing
the storax in warm water until it becomes more liquid, and then pour it
in very thin threads into the flask. Shake frequently.
_Myrrh tincture._--Myrrh 1 lb., best quality of alcohol 2 quarts.
_Musk-seed or abelmosk tincture._--Abelmosk grains 21 ozs., best
quality of alcohol 2½ quarts.
Reduce the grains to a fine powder, bring the powder into a bottle,
and add the alcohol. This _tincture abelmoschi_ fulfils its object as
a fixing agent only when about one year old, when it possesses a very
fine aroma.
Abelmosk grains are the seeds of a plant (_Abelmoschus moschatus
Mönch_; _Hebiscus abelmoschus, L._) indigenous to Central Africa,
Arabia, and India. They are reddishgray, kidney-shaped, slightly
corrugated on the surface, and of an agreeable musk-like odor. The
substance producing the musk odor lies in the seed coat. The odor
becomes very pronounced on rubbing the seeds between the hands.
_Angelica root tincture._--Angelica root 16 ozs., best quality of
alcohol 2 quarts.
Bruise or rasp the root, bring it into a bottle, add the alcohol, and
shake frequently.
_Orris-root tincture._--Pulverized orris root of best quality 2 lbs.,
alcohol of best quality 3 quarts.
Pulverize the root, bring it into a glass flask, and add the alcohol.
The powder having a great tendency to ball together, it is necessary
to shake five or six times daily, and continue to do so for 14 days.
In straining off the tincture, it is advisable to bring the entire
contents of the flask upon a close linen cloth stretched over a tin
vessel. The orris-root powder remaining upon the cloth after the
tincture has run off is returned to the flask, and fresh alcohol added
in order to obtain a second extract.
_Musk-root_ or _sumbul-root tincture_.--Sumbul root 1 lb., best quality
of alcohol 2½ quarts.
Proceed in the same manner as given under angelica-root tincture.
_Tonka-bean tincture._--Tonka beans 8 ozs., alcohol of best quality 3
pints.
The tonka bean is of great importance for perfumery. The tincture
prepared from it has an agreeable, penetrating odor, and in mixing it
with other odors, great care has to be exercised, so that the tonka
odor is not too prominent. The tincture is prepared as follows: Bring
the beans, without comminuting them or removing the white coating
adhering to them, into a flask, add the alcohol, and let the whole
macerate, with frequent shaking, for about 14 days. Then filter off the
fluid. The tincture prepared in this manner only contains the cumarin
found as a white coating upon the beans, and is used only for the
finest products. Now take the beans from the flask, comminute them,
return them to the flask, and add 1¼ quarts of alcohol. This extract
gives an excellent tincture suitable for products of medium quality.
_Cumarin tincture._--Cumarin 5½ drachms, best quality of alcohol 1
quart.
_Heliotropin tincture._--The white crystals of heliotropin yield
with alcohol a solution clear as water, which is much used in the
preparation of _Extrait héliotrope_.
_Vanilla tincture._--Best quality of Bourbon vanilla 5¼ ozs., alcohol
of best quality 2 quarts.
To prepare the tincture proceed as follows: Cut the so-called vanilla
pods lengthwise and then into as small pieces as possible, and bring
the latter together with the alcohol into a flask. Some perfumers
triturate the commimuted vanilla with sugar in a porcelain mortar,
whereby the small-seed bodies contained in the pod are ground up, and
a better yield is claimed to be obtained. Though by this trituration
a tincture of a darker color may be obtained, the color alone is by
no means a proof of the strength of the tincture. Care must be had to
bring the white, downy crystals of vanillin found upon the vanilla pods
into the flask.
_Vanillin tincture._--Vanillin 1½ drachms, alcohol 2 quarts.
_Vitivert tincture._--Vitivert rhizome 8 ozs., best quality of alcohol
2 quarts.
Reduce the rhizome to as fine a powder as possible, bring the latter
into a flask, add the alcohol and shake frequently.
_Juniper-berry tincture._--Juniper berries 2 lbs., best quality of
alcohol 5 pints.
The juniper berries (the fruits of _Juniperus communis, L._) are
comminuted, and the alcohol is poured over them.
_Patchouli extract._[15]--Patchouli leaves 1 lb., best quality of
alcohol 5 pints.
[15] Compare patchouli oil, p. 130.
Bring the pulverized leaves into a bottle and add the alcohol. The
tincture from patchouli leaves being dark-green is not suitable for
the preparation of _Extraits_, since white substances are colored
grass-green by it; only traces of the tincture may be used for the
purpose of giving the _Extrait patchouli_ a greenish shade of color.
The tincture may, however, be utilized for milled patchouli soaps.
From many of the above-mentioned perfume-substances, which serve
for the preparation of tinctures and are not entirely soluble in
alcohol, but leave a residue after extraction, a second infusion may
be made. Musk, castor, and the resins dissolve completely, there
remaining behind only the impurities and any mineral constituents
present which possess no aroma. But all residues from woods, fruits,
etc., are suitable for a second extraction, most of the tinctures
thus obtained being quite aromatic, and, as will be seen later on in
giving receipts, can be very advantageously utilized. For the second
extraction less alcohol has to be taken than for the first.
Since many perfumers consider it of greater advantage and more suitable
to first dissolve the volatile oils used for the _Extraits d'Odeurs_,
and to prepare a tincture in this manner, several receipts for the
purpose are given below. In the receipts for perfumery given in the
next following sections, the volatile oils are specified as such, and
not as tinctures, because the _Extraits d'Odeurs_ containing evidently
much non-saturated alcohol, the volatile oils will in time completely
dissolve in them. An exception to this rule might be ylang-ylang oil
and perhaps orris-root oil. Ylang-ylang oil is soluble with difficulty,
even in very strong alcohol, and if directly used for the _Extrait_,
the latter remains turbid for weeks, and frequently, especially in
winter, does not become clear, notwithstanding repeated filtering.
However, by preparing in good time an ylang-ylang tincture this evil is
avoided.
_Almond-oil (bitter) tincture._--Bitter almond oil 2¾ drachms,
alcohol[16] 1 quart.
[16] For all the tinctures, 95 to 97 per cent. alcohol of the best
quality is to be used.
_Balm-oil tincture._--Balm oil 5½ drachms, alcohol 1 quart.
_Basil-oil tincture._--Basil oil 14 drachms, alcohol 1 quart.
_Bergamot-oil tincture._--Bergamot oil 3½ ozs., alcohol 4 quarts.
_Canango-oil tincture._--Canango oil (Java), 1¾ ozs., alcohol 1
quart.
_Cassia-oil tincture._--Cassia oil 1¾ ozs., alcohol 1 quart.
_Cedar-oil tincture._--Cedar oil 1 oz., alcohol 1 quart.
_Cinnamon-oil tincture._--Ceylon cinnamon oil 5½ drachms, alcohol 1
quart.
_Citronella-oil tincture._--Citronella oil 1 oz., alcohol 1 quart.
_Clove-oil tincture._--Oil of cloves 11 drachms, alcohol 1 quart.
_Eucalyptus-oil tincture._--Eucalyptus oil 1 oz., alcohol 1½ quarts.
_Geranium-oil tincture._--Palma rosa oil 14 drachms, alcohol 1 quart.
_Lavender-oil tincture._--Lavender oil 1¾ ozs., alcohol 1 quart.
_Lemon-grass-oil tincture._--Lemon-grass oil 1 oz., alcohol 1 quart.
_Lemon-oil tincture._--Oil of lemons 1¾ ozs., alcohol 1 quart.
_Licari-oil tincture._--Licari oil 5½ drachms, alcohol 1 quart.
_Myrrh-oil tincture._--Myrrh oil 5½ drachms, alcohol 1 quart.
_Neroli-oil tincture._--Neroli oil 5½ drachms, alcohol 1 quart.
_Opopanax-oil tincture._--Opopanax oil 5½ drachms, alcohol 1 quart.
_Orris-root-oil tincture._--Orris-root oil 5½ drachms, alcohol 1 quart.
_Patchouli-oil tincture._--Patchouli oil 5½ drachms, alcohol 1 quart.
_Petit-grain-oil tincture._--Petit-grain oil 11 drachms, alcohol 1
quart.
_Pine-leaf-oil tincture._--Pine-leaf oil[17] 14 drachms, alcohol 1
quart.
[17] By pine-leaf oil is understood pine oil or dwarf-pine oil. See p.
149.
_Portugal-oil tincture._--Portugal oil 1¾ ozs., alcohol 1 quart.
_Sandal-wood-oil tincture._--Sandal-wood[18] oil 5½ drachms, alcohol 1
quart.
[18] The better quality of oil from the East Indian wood is to be used.
_Verbena-oil tincture._--Verbena oil 11 drachms, alcohol 1 quart.
_Vitivert-oil tincture._--Vitivert oil 2¾ drachms, alcohol 1 quart.
_Wintergreen-oil tincture._--Wintergreen oil 5½ drachms, alcohol 1
quart.
_Ylang-ylang-oil tincture._--Ylang-ylang oil 11 drachms, alcohol 3
quarts.
_Rose-oil tincture._--Rose oil (Turkish)[19] 1¾ ozs., alcohol 6½
quarts.
[19] Bulgarian rose oil is generally designated "Turkish rose oil."
Rose oil, if directly added to the alcohol, dissolves with difficulty
and incompletely. By the following method the object is, however,
readily accomplished:--
Bring about 5½ ozs. of pulverized sugar into a capacious porcelain
mortar, add the rose oil and mix intimately with the pestle. Then pour
the thickly-fluid mass through a glass funnel into a glass flask and
rinse the mortar with alcohol until the prescribed 6½ quarts of the
latter have been brought into the flask. Frequent shaking accelerates
the complete solution of the rose oil.
EXTRAITS AUX FLEURS. We now proceed to give receipts for _Extraits
d'Odeurs_, and consider first the flower odors, _Extraits aux fleurs_.
_By extracts are thereby understood the odors extracted from French
flower pomades._ Any coloring matter required is mentioned under the
respective receipts.
Great care has to be exercised in the preparation of _Extraits_ and
_Bouquets_, and special attention must be paid that they actually
represent the odor whose name they bear.
_Extrait acacia._--Extract No. 1 from _Pomm. Acacia_ 750 drachms,
bergamot oil 1, lavender oil 1, eucalyptus oil ½, orris-root tincture
125, musk-root tincture 12½, ambergris tincture 2½, civet tincture 1,
musk tincture 1.
_Extrait cassie._--Extracts No. 1 from _Pomm. Cassie_ 500 drachms,
from _Pomm. Tubereuse_ 125, bergamot oil 5, orris-root tincture 75,
tinctures of vitivert and angelica each 12½, tinctures of musk and
ambergris each 2½.
_Extrait héliotrope_ (_Receipt No. 1_).--Extracts No. 1 from _Pomm.
Héliotrope_ 750 drachms, and from _Pomm. Rose_ 75, bergamot oil 2½,
rose-geranium oil 1½, musk tincture 2½, civet tincture 1½, heliotropin
tincture 50.
_Extrait héliotrope_ (_Receipt No. 2_).--Extracts No. 1 from _Pomm.
Héliotrope_ 500 drachms, and from _Pomm. Rose_ and _Pomm. Orange_ 50
each, bergamot oil 5, clove oil 2½, vanilla tincture 50, orris-root
tincture 100, musk-root tincture 25, tinctures of musk and civet 5
each, benzoin tincture 10, Peru-balsam tincture 5.
_Extrait jacinthe._--Extracts No. 1 from _Pomm. Jacinthe_ 750 drachms,
and from _Pomm. Acacia_ 100; bergamot oil 5, clove oil 1, storax
tincture 2½, musk-root tincture 12½, tinctures of musk and ambergris 1½
each.
_Extrait jasmin._--Extracts No. 1 from _Pomm. Jasmin_ 500 drachms,
and from _Pomm. Orange_ 100; civet tincture 1½, ambergris tincture 1,
sandal-wood oil 3 drops.
_Essence of the odor of linden blossoms._--Extracts No. 1 from _Pomm.
Acacia_ 250 drachms, from _Pomm. Jasmin_ 50, and from _Pomm. Jonquille_
100; pure camomile oil 1½, oil of lemons 2½, ambergris tincture 5,
civet tincture 3.
_Extrait jonquille._--Extract No. 1 from _Pomm. Jonquille_ 750 drachms,
lavender oil ½, bergamot oil 2½, Ceylon cinnamon oil ½, storax
tincture 1½, tinctures of abelmosk and angelica each 5, musk tincture
1½, civet tincture 1.
_Extrait magnolia._--Extracts No. 1 from _Pomm. Tubereuse_ 150 drachms,
from _Pomm. Acacia_ 250, and from _Pomm. Rose_ 125, balm oil 2½,
tinctures of vanilla and cumarin each 12½, civet tincture 1½, musk
tincture 2½.
_Extrait muguet_ (_lily of the valley_).--Extracts No. 1 from _Pomm.
Jonquille_ 750 drachms, from _Pomm. Jasmin_ 100, from _Pomm. Tubereuse_
200, and from _Pomm. Acacia_ and _Pomm. Orange_ each 100; bergamot oil
7½ drachms, oil of lemons 2½, angelica oil 3 drops, storax tincture 5
drachms, musk tincture 2½, vanilla tincture 5, ambergris tincture 2,
ylang-ylang tincture 100, wintergreen tincture 25, bitter-almond-oil
tincture 2½.
_Extrait fleurs de Mai_ (_May flowers_).--Extract No. 1 from _Pomm.
Réséda_, _Pomm. Rose_ and _Pomm. Héliotrope_, each 75 drachms; from
_Pomm. Jasmin_ 125, and from _Pomm. Orange_ 50; bergamot oil 7½, Ceylon
cinnamon oil 2½, orris-root tincture 50, tinctures of ambergris and
musk, each 15, ylang-ylang tincture 25.
_Extrait ixora._--Extracts No. 1 from _Pomm. Tubereuse_ 125 drachms,
from _Pomm. Cassie_ and _Pomm. Réséda_, each 175; bergamot oil 5,
orris-root tincture 125, musk tincture 10, benzoin tincture 25.
_Extrait Orange._--Extracts No. 1 from _Pomm. Orange_ 500 drachms, from
_Pomm. Acacia_ 100; Portugal oil 7½, tinctures of musk and ambergris,
each 1.
_Extrait white rose._--Rose-oil tincture from Turkish rose oil 500
drachms, bergamot oil 1¼, sandal-wood oil 3 drops, nutmeg oil 1 drop,
musk tincture ¾ drachm, civet tincture ½ drachm.
_Extrait rose v. d. centifolie._--Extract No. 1 from _Pomm. Rose_ 500
drachms, rose-oil tincture from Turkish rose oil 500, rose-geranium oil
10, musk tincture, 2½, sandal-wood oil, 7 drops.
_Extrait violette._--Extracts No. 1 from _Pomm. Violette_ 500 drachms,
and from _Pomm. Cassie_ 250; orris-root tincture 125, musk tincture 1½,
sandal-wood oil 3 drops.
To give the _extrait violette_ an apparently greater concentration,
it is compounded with a green coloring tincture. The latter may be
prepared by bringing comminuted dried spinach leaves into a bottle and
pouring 96 per cent. alcohol over them. The result is a handsome green
coloring matter; but care must be taken not to add too much of it to
the _extrait_, as otherwise it might stain the handkerchief, etc.[20]
[20] This spinach extract unfortunately bleaches very rapidly
when exposed to light, and the extraits colored with it acquire
a dirty-brown color. Hence it is recommended to use the "green
tincture," which can be purchased from the larger manufactories of
volatile oils.
_Extrait de violette de Parme._--Extract No. 1 from _Pomm. Violette_
750 drachms, orris-root oil and bergamot oil each 2½, tinctures of
musk, ambergris, and bitter-almond oil each 1½.
This _extrait_ may also be colored slightly green.
_Extrait tubereuse._--Extract No. 1 from _Pomm. Tubereuse_ 500 drachms,
bergamot oil 2½, Ceylon cinnamon oil ½, musk tincture 1½, storax
tincture 2½.
_Extrait réséda._--Extracts No. 1 from _Pomm. Réséda_ 750 drachms, and
from _Pomm. Violette_ 100; bergamot oil 7½, rose-geranium oil 2½, clove
oil 1½, musk tincture 2, ambergris tincture 1.
A trace of the above-mentioned green coloring substance may be added.
_Extrait ylang-ylang._--Extracts No. 1 from _Pomm. Jasmin_, _Pomm.
Jonquille_, _Pomm. Orange_, and _Pomm. Acacia_, each 250 drachms,
bergamot oil 7½, angelica oil 2½, ylang-ylang tincture 500, abelmosk
tincture 25, tonka-bean extract 7½, musk tincture 4, ambergris tincture
2½.
COMPOUND ODORS (BOUQUETS). _Extrait Edelweiss._--Extracts No. 1 from
_Pomm. Jasmin_ and _Pomm. Tubereuse_ 250 drachms each, and from
_Pomm. Orange_, _Pomm. Héliotrope_, and _Pomm. Jacinthe_ 125 each,
bergamot oil 10, basil oil 5, tinctures of musk and ambergris each 5,
bitter-almond-oil tincture 2½, tinctures of angelica and vitivert each
25.
_Extrait ess-bouquet._--Extracts No. 1 from _Pomm. Acacia_ and _Pomm.
Cassie_ each 100 drachms, from _Pomm. Jasmin_ 325, from _Pomm. Rose_
75, and from _Pomm. Orange_ 250; bergamot oil 40, Ceylon cinnamon oil
and clove oil each 5, French rose-geranium oil 10, sandal-wood oil 2½,
licari oil 8, rose-oil tincture from Turkish rose oil 75, orris-root
tincture 50, tinctures of ambergris and civet each 10, musk tincture
15, musk-root tincture 37½, benzoin tincture 15.
_Extrait spring flower._--Extracts No. 1 from _Pomm. Jasmin_, _Pomm.
Cassie_, _Pomm. Orange_, _Pomm. Jonquille_, _Pomm. Tubereuse_, and
_Pomm. Violette_ each 100 drachms, from _Pomm. Rose_ 50, from _Pomm.
Réséda_ 100, and from _Pomm. Héliotrope_ and _Pomm. Acacia_ each 50;
neroli oil 2½, bergamot oil 5, vitivert oil ½, rose-oil tincture from
Turkish rose oil 50, musk-root tincture 12½, musk tincture 5, civet
tincture 2½, orris-root tincture 25.
_Extrait bouquet Eugenie._--Extracts No. 1 from _Pomm. Cassie_ 100
drachms, from _Pomm. Tubereuse_ 75, from _Pomm. Jasmin_ 125; bergamot
oil 10, licari oil 2½, rose-oil tincture from Turkish rose oil 75,
musk-root tincture 10, cumarin tincture 7½, orris-root tincture 75,
tinctures of angelica and musk each 10, ambergris tincture 5.
_Extrait excelsior._--Extracts No. 1 from _Pomm. Jasmin_ 200 drachms
and from _Pomm. Orange_ and _Pomm. Héliotrope_ each 100; oils of lemon
and rose geranium each 4, rose-oil tincture from Turkish rose oil 60,
orris-root tincture 50, musk tincture 5, abelmosk tincture 10, opopanax
tincture 5, storax tincture 1.
_Extrait Frangipani._--Extracts No. 1 from _Pomm. Cassie_ 150 drachms,
and from _Pomm. Jasmin_ 50; French rose geranium oil 5, cassia oil 2,
licari oil 3, sandal-wood oil 1, orris-root tincture 100, angelica
tincture 8, musk tincture 5, storax tincture 5.
_Extrait jockey club._--Extracts No. 1 from _Pomm. Orange_ 150 drachms,
from _Pomm. Rose_ 35, from _Pomm. Jasmin_ 150, and from _Pomm.
Jonquille_ and _Pomm. Héliotrope_ each 30; bergamot oil 8, Ceylon
cinnamon oil 2, Portugal oil 6, cedar oil 1, clove oil 2, tincture of
rose oil from Turkish rose oil and of orris root each 40, musk-root
tincture 8, musk tincture 10, ambergris tincture 3, vanilla tincture 5.
_Extrait opopanax._--Extracts No. 1 from _Pomm. Orange_ 250 drachms,
and from _Pomm. Héliotrope_ 125; opopanax oil 10, Ceylon cinnamon oil
5, rose-oil tincture from Turkish rose oil 125, opopanax tincture 25,
orris-root tincture 62½, musk tincture 4, ambergris tincture 5.
_Extrait patchouly._--Extract No. 1 from _Pomm. Acacia_ 100 drachms,
patchouli oil 4, clove oil and Portugal oil, each 2, rose-oil tincture
from Turkish rose oil 40, orris-root tincture 30, musk-root tincture
10, vitivert tincture 10, patchouli tincture 1.
_Extrait millefleurs._--Extracts No. 1 from _Pomm. Jasmin_ 250 drachms,
from _Pomm. Jonquille_ 100, _Pomm. Rose_ 75, _Pomm. Acacia_ 100,
_Pomm. Orange_ and _Pomm. Tubereuse_ each 150, and _Pomm. Cassie_ 100;
bergamot oil 20, rose geranium oil and Portugal oil each 15, oils
of angelica and sandal wood, each 5, rose-oil tincture from Turkish
rose oil 150, orris-root tincture 250, vanilla tincture 15, musk-root
tincture 35, tolu-balsam tincture 10, tinctures of storax and patchouli
each 5, musk tincture 30, civet tincture 25.
_Extrait bouquet Victoria._--Extracts No. 1 from _Pomm. Rose_ 200
drachms, _Pomm. Orange_ and _Pomm. Tubereuse_, each 100, _Pomm.
Jasmin_ 300, and _Pomm. Héliotrope_ 200; lemon oil 20, verbena oil
5, French rose geranium oil 10, musk tincture 20, tinctures of civet
and ambergris each 5, musk-root tincture 40, tolu-balsam tincture 20,
orris-root tincture 150.
_Extrait kiss-me-quick._--Extracts No. 1 from _Pomm. Acacia_ and _Pomm.
Jonquille_ each 100 drachms, and _Pomm. Jasmin_ 40; bergamot oil 4, oil
of lemons 2, rose-oil tincture from Turkish rose oil 30, tinctures of
vitivert and angelica 8, ambergris tincture 4, civet tincture 2, musk
tincture 1.
_Extrait mogadore._--Extracts No. 1 from _Pomm. Jasmin_ 100 drachms,
from _Pomm. Jonquille_ and _Pomm. Acacia_, each 50, from _Pomm. Orange_
40; bergamot oil 6, oil of lavender 1, French rose geranium oil 2,
tinctures of musk, ambergris, tolu balsam, and cumarin, each 10,
tincture of orris root 50.
_Extrait bouquet Prince Albert._--Extracts No. 1 from _Pomm. Jasmin_
150 drachms, from _Pomm. Tubereuse_, _Pomm. Orange_, and _Pomm. Cassie_
each 50, _Pomm. Rose_ 25, neroli oil 2, bergamot oil 4, musk tincture
2, tonka bean extract 4, angelica tincture 10, ambergris tincture 2.
_Extrait musc._--Extracts No. 1 from _Pomm. Orange_, _Pomm.
Héliotrope_, and _Pomm. Cassie_ each 50 drachms; clove oil 4, cassia
oil 2, tinctures of abelmosk and musk-root each 10, opopanax tincture
4, musk tincture 30, civet tincture 5, orris-root tincture 50.
_Extrait new-mown hay._--Extracts No. 1 from _Pomm. Réséda_ 200
drachms, _Pomm. Rose_ 40, _Pomm. Cassie_ 80, _Pomm. Acacia_ 40; French
rose geranium oil 4, bergamot oil 10, myrrh oil 5, tonka-bean extract
30, vitivert tincture 10, musk-root tincture 16, benzoin tincture 4.
_Extrait chypre._--Extracts No. 1 from _Pomm. Orange_ 60 drachms,
_Pomm. Jasmin_ 40, _Pomm. Cassie_ 110, _Pomm. Héliotrope_ 40; French
rose geranium oil 6, bergamot oil 2, cedar oil ⅗, benzoin tincture 4,
orris-root tincture 30, musk tincture 5, civet tincture 4, abelmosk
tincture 10.
_Extrait maréchal._--Extracts No. 1 from _Pomm. Héliotrope_ and _Pomm.
Orange_ each 200 drachms, from _Pomm. Jasmin_ 75; oils of sandal wood
and cloves each 5, Portugal oil 10, cedar oil 1, rose-oil tincture from
Turkish rose oil 100, orris-root tincture 75, vitivert tincture 25,
civet tincture 10, musk tincture 20, bitter almond oil tincture 1½.
_Extrait mousseline._--Extracts No. 1 from _Pomm. Jasmin_ 250 drachms,
_Pomm. Rose_ 150, and _Pomm. Jonquille_, _Pomm. Héliotrope_, and _Pomm.
Cassie_, each 125; French rose geranium oil 12½, oil of cloves 10,
cassia oil 5, wintergreen oil 1, orris-root tincture 125, rose-oil
tincture from Turkish rose oil 100, musk tincture 12½, civet tincture
10, vitivert tincture 37½, abelmosk tincture 25.
In compiling the abundant choice of receipts for _Extraits d'Odeurs_
given above, the golden mean has been chosen in regard to the quality
of these odors, they, when carefully prepared, giving, at a moderate
cost of manufacture, a product which in most cases will satisfy the
demands of lovers of perfumes. To enable the perfumer, however, to
satisfy the highest demands attention is called to, and a brief
explanation given of, the so-called "_Extraits triple concentrés_."
For the preparation of these stronger products, the employment of
a stronger foundation, _i. e._, of more highly saturated extracts
from French flower pomades, is required. For this purpose the French
perfumers prepare, under No. 30, flower pomades of all odors which are
exclusively used for concentrated _Extraits_. They are, of course,
correspondingly higher in price than those prepared from No. 18, which
have previously been treated of.
The method of preparing the extracts from these pomades, No. 30, is the
same as previously described, the proportion of pomade to alcohol being
also the same; hence for 2 lbs. of pomade 1¾ quarts of alcohol are
to be used.
The proportions of volatile oils and tinctures given in the above
receipts are also to be retained. The stronger extracts from the flower
pomades are the only measure in the preparation of the _Extraits
triple concentrés_, and such must be the case since the object of the
concentration of the _Extraits_ is thus completely attained by the
greater prominence of the flower odors from the _Extraits d'Odeurs_.
For the preparation of _Extraits d'Odeurs_, the French perfumers also
manufacture a concentrated flower extract of the various odors. This
extract is simply dissolved in alcohol, the solution being effected
immediately, so that this method of preparing _Extraits d'Odeurs_ is
the simplest imaginable. However, the price of such extract (1000
francs = $200 and more per kilogramme = 2.2 lb.) is a considerable
item, so that most perfumers will prefer the extracts from the flower
pomades as previously described.
EXTRAITS D'ODEURS, QUALITY II.--In addition to the _fine_ extracts
given in the preceding section, a small selection of quite cheap
receipts for quality II of such extracts is here given, the extracts
No. 2 offering sufficient material for their preparation. In the
introduction to the previous section, attention has been called to
the fact that quite useful tinctures may be prepared from substances
leaving behind solid residues, there being also on hand the second
extract from the flower pomades.
Besides the alcohol, such tinctures and extracts cost only the small
trouble of treatment. For this second quality only half the quantity of
volatile oils prescribed for the best quality is used. Such tinctures,
from which a second extract cannot be had, may, for this purpose, be
diluted one-half with alcohol, which need not be of the best quality,
thus preparing a second quality of them.
The process to be followed is illustrated by a selection from the first
_Extrait_ receipts which have been converted into _Extraits_ of quality
II.
_Extrait violette II._--Extracts No. 2 from _Pomm. Violette_ 500
drachms, from _Pomm. Cassie_ 250; bergamot oil 2½, musk tincture No.
2, 1½, ambergris tincture No. 2, ¾, diluted with alcohol ¾, bitter
almond oil tincture No. 2, 1, orris-root tincture No. 2, 125.
Add a small quantity of green coloring substance.
_Extrait rose II._--Extract No. 2 from _Pomm. Rose_ 500 drachms,
African rose geranium oil 4, sandal-wood oil 3 drops, musk tincture
No. 2, 2½ drachms, rose-oil tincture from Turkish rose oil 250 drachms
diluted with an equal quantity of alcohol, which may be called rose
tincture No. 2.
_Extrait réséda II._--Extracts No. 2 from _Pomm. Réséda_ 750 drachms
and from _Pomm. Violette_ 100, bergamot oil 3½, African rose-geranium
oil 1, clove oil 1, musk tincture No. 2, 2, ambergris tincture ½
diluted with alcohol ½.
_Extrait ylang-ylang II._--Extracts No. 2 from _Pomm. Jasmin_, _Pomm.
Jonquille_, _Pomm. Orange_, and _Pomm. Acacia_ each 250 drachms;
bergamot oil 3½, angelica oil 1¼, ylang-ylang tincture 250 diluted
with the equal quantity of alcohol, abelmosk No. 2, 25, tonka-bean
extract No. 2, 7½, musk tincture No. 2, 4, ambergris tincture 1¼
diluted with the same quantity of alcohol.
_Extrait new-mown hay II._--Extracts No. 2 from _Pomm. Réséda_ 500
drachms, from _Pomm. Rose_ 100, from _Pomm. Cassie_ 200 and _Pomm.
Acacia_ 100; palma rosa oil 5, bergamot oil 12½, myrrh oil 6,
tonka-bean extract No. 2, 75, vitivert tincture No. 2, 25, musk-root
tincture No. 2, 40, benzoin tincture 5 diluted with the same quantity
of alcohol.
_Extrait chypre II._--Extracts No. 2, from _Pomm. Orange_ 150 drachms,
from _Pomm. Jasmin_ 100, _Pomm. Cassie_ 275, and _Pomm. Héliotrope_
100; palma rosa oil 7½, bergamot oil 2½, cedar oil ¾, orris-root
tincture No. 2, 75, musk tincture No. 2, 12½, abelmosk tincture No. 2,
25, civet tincture 5 diluted with alcohol 5, benzoin tincture 5 diluted
with alcohol 5.
_Extrait ess. bouquet II._--Extracts No. 2 from _Pomm. Acacia_ and
_Pomm. Cassie_ each 100, from _Pomm. Jasmin_ 375, _Pomm. Rose_ 75,
_Pomm. Orange_ 250; bergamot oil 20, Ceylon cinnamon oil and clove oil
each 2½, African rose geranium oil 5, sandal-wood oil 1¾, licari oil
2, rose-oil tincture from Turkish rose oil 37½ diluted with an equal
quantity of alcohol, orris-root tincture No. 2, 50, ambergris tincture
5 diluted with an equal quantity of alcohol, civet tincture 5 diluted
with an equal quantity of alcohol, musk tincture No. 2, 15, musk-root
tincture No. 2, 37½, benzoin tincture 7½ diluted with an equal quantity
of alcohol.
_Extrait muguet II._--Extracts No. 2 from _Pomm. Jonquille_ 750
drachms, _Pomm. Jasmin_ 100, _Pomm. Tubereuse_ 200 and _Pomm. Acacia_
and _Pomm. Orange_ each 100; bergamot oil 3½, oil of lemons 1¼,
angelica oil 2 drops, storax tincture 2½ drachms diluted with an
equal quantity of alcohol, musk tincture No. 2, 2½, vanilla tincture
5, ambergris tincture 1, diluted with an equal quantity of alcohol,
ylang-ylang tincture 50 diluted with alcohol 50, wintergreen tincture
12½ diluted with alcohol 12½, bitter-almond oil 1¼ diluted with alcohol
1¼.
_Extrait bouquet Victoria II._--Extracts No. 2 from _Pomm. Rose_ 100
drachms, _Pomm. Orange_ and _Pomm. Tubereuse_ each 50; _Pomm. Jasmin_
150, _Pomm. Héliotrope_ 100; lemon oil 5, verbena oil 1½, African rose
geranium oil 2½, musk tincture No. 2, 10, musk-root tincture No. 2, 20,
orris-root tincture No. 2, 75, civet tincture 1¼ diluted with alcohol
1¼, ambergris tincture 1¼ diluted with alcohol 1¼, tolu-balsam tincture
5 diluted with alcohol 5.
_Extrait spring flower II._--Extracts No. 2 from _Pomm. Jasmin_,
_Pomm. Cassie_, _Pomm. Orange_, _Pomm. Jonquille_, _Pomm. Tubereuse_
and _Pomm. Violette_, each 100 drachms, from _Pomm. Rose_ 50, _Pomm.
Réséda_ 100, and _Pomm. Héliotrope_ and _Acacia_, each 50; neroli
oil 1¼, bergamot oil 2½, vitivert oil 13 drops, rose-oil tincture
from Turkish rose oil 25 drachms, diluted with alcohol 25, musk-root
tincture No. 2, 12½, musk tincture No. 2, 12½, orris-root tincture No.
2, 25, civet tincture 1¼ diluted with alcohol 1¼.
_Extrait ixora II._--Extracts No. 2 from _Pomm. Tubereuse_ 125 drachms,
from _Pomm. Cassie_ and _Pomm. Réséda_ each 175; bergamot oil 2½,
orris-root tincture No. 2, 125, musk tincture No. 2, 10, benzoin
tincture 12½ diluted with alcohol 12½.
_Extrait Frangipani II._--Extracts No. 2 from _Pomm. Cassie_ 375
drachms, and _Pomm. Jasmin_ 125; African rose geranium oil 12, cassia
oil 2½, licari oil 3½, sandal-wood oil 1¼, orris-root tincture No. 2,
250, angelica tincture No. 2, 20, musk tincture No. 2, 12½, storax
tincture 6 diluted with alcohol 6½.
_Cologne water, eau de Cologne._--Owing to its excellent properties,
Cologne water is, without doubt, one of the most popular perfumes.
It was invented early in the eighteenth century, and is perhaps the
only perfume which has kept its reputation for so long a time. It was
formerly employed as a medicine in all imaginable diseases, and even
now is in some cases successfully used in slight ailments, such as
headache, nausea, etc.
The success and reputation of Cologne water are the natural results
of a good product prepared with a thorough knowledge of the subject.
However, in order to be enabled to impart to Cologne water its
generally known excellent qualities, it is necessary to have a thorough
knowledge of the materials used, as well as to understand the method of
fabrication, and the proper treatment of all.
For the preparation of actually good Cologne water employment of the
best materials is the first condition. The alcohol must be pure, _i.
e._, free from fusel oil, and 95 to 96 per cent. strong, so as to
effect a ready and complete solution of the volatile oils. The latter
also should be of the best quality and proper age, _i. e._, neither
too young nor too old. If too young or too recently distilled, the
aroma is not thoroughly developed, and if, on the other hand, too
old, they have lost the greater portion of their aroma, are thickly
fluid, acquire a dark coloration, and are finally converted into a
resinous substance in which condition they are entirely unfit for finer
products. A cool and dry cellar is required for storing volatile oils,
and they must also be protected from air and sunlight.
Regarding the durability of the volatile oils used in the preparation
of Cologne water, the following may be said:--
_Bergamot oil_ is quite durable; in well-closed bottles stored in a
cool cellar it keeps quite well for 3 to 4 years. _Oil of lemons_ is,
however, very sensitive, and has to be especially protected against
heat, by which it is readily decomposed and, so to say, turns sour.
Freshly-distilled _neroli oil_ should never be used, it acquiring its
proper aroma only after being stored for about 2 years; on the other
hand, it should not be too old. When 6 to 8 years old, it shows a
tendency to rancidity, which can, however, be prevented by mixing it at
the proper time with an equal quantity of alcohol of the best quality.
_Petit-grain oil_ is apt to spoil when kept for several years, and
hence it is not advisable to have too large a supply of it on hand.
Besides the French variety of this volatile oil, there has existed for
several years past another kind, namely the _Paraguay petit-grain oil_,
which is about one-half cheaper than the French. While some consider
both oils as equally good, the French product no doubt deserves the
preference. Of _lavender oil_ only the best French oil, especially made
in France for the preparation of _Eau de Cologne_, should be used. The
price of the English Mitcham lavender oil, being six times that of
the French oil, is simply excessive. Of _rosemary oil_, an especially
fine quality for Cologne water, which can be highly recommended, is
also manufactured in France. Of _balm oil_ only the best German product
should be taken. The three varieties of volatile oils last mentioned
keep for years, especially when kept in hermetically-closed bottles in
a cool place protected from the sun.
Rose water and orange-blossom water also need careful treatment, the
bottles containing them requiring to be well stoppered and kept in a
cool place. These waters being liable to spoil, the supply of them
should be renewed from year to year. As regards the compounding of
the volatile oils, it is advisable to mix them in a capacious glass
flask, add at least an equal weight of alcohol of the best quality,
shake thoroughly, let the mixture stand about 14 days, and then in the
apparatus incorporate it with the required quantity of alcohol.
When the alcohol and volatile oils are intimately mixed, the mixture
is allowed to stand quietly for about 14 days, when solution of the
volatile oils will be complete. Now add, with vigorous agitation,
the rose water and the orange-blossom water, and let the whole stand
quietly to become clear.
Cologne water thus carefully prepared answers all demands. Special
attention is here called to the fact that all manipulation by the
addition of fixing or conspicuous substances is injudicious. An
addition of tincture of musk or civet should particularly be avoided.
Nervous people immediately detect such additions, even if present only
in very small quantities, and in most cases refuse the Cologne water
containing them.
Experience having shown that all alcoholic perfumes develop their
proper aroma only after storing for some time, provision must be made
to have always a sufficient supply of Cologne water on hand. It is best
to keep it in large glass balloons in a cool cellar. Wooden vessels
are impracticable on account of their permeability and other evils.
Metallic vessels, if used, should be tinned. Vessels defective in this
respect, or tinned with tin containing lead, exert an injurious effect
upon the aroma of the water. In the latter case, lead is dissolved,
even if only in small quantities, and a dirty precipitate injurious to
the odor of the Cologne water is formed.
The filtering of the Cologne water is best effected through white
filtering paper and a glass funnel; the paper, however, should not
have been bleached with chlorine, the odor of the latter being readily
perceived and having an injurious effect upon the aroma of the water.
Filtering should be avoided as much as possible by carefully decanting
off the clear water and filtering the sediment only. Filtering through
charcoal, magnesia, or other clarifying agents, should not be made use
of for fine perfumes, their odor being injured by all such means.
In the following a selection of receipts for Cologne water is given;
it is, however, especially mentioned that only good, pure materials
must be used even for the inferior qualities. A receipt for the now
fashionable "Maiglöckchen Eau de Cologne" is also given.
_Cologne water, quality I._--Bring into a large glass balloon 95 to
96 per cent. alcohol of the best quality 7.9 gallons, lemon oil 14.11
ozs., bergamot oil 15, neroli oil 4.23, French extra lavender oil 1.05
oz., rosemary oil 0.7, best German balm oil 0.42; mix thoroughly, and
after 14 days add best orange-blossom water and rose water each 2.64
quarts. Mix again thoroughly, and then let stand until wanted for use.
_Cologne water, quality II._--Bring into a large glass balloon 95 to
96 per cent. alcohol of the best quality 7.9 gallons, lemon oil 10.58
ozs., bergamot oil 12.34, neroli oil 1.76, French extra lavender oil
0.8, rosemary oil 0.63, finest German balm oil 0.35, French petit-grain
oil 0.8; mix thoroughly, and after 14 days add best orange-blossom
water and rose water each 2.64 quarts. Mix again thoroughly, and then
let stand until wanted for use.
_Cologne water, quality III._--Bring into a large glass balloon 95 to
96 per cent. alcohol of the best quality 7.9 gallons, lemon oil 7.05
ozs., bergamot oil 7.94, Portugal oil 3.52, French petit-grain oil
1.58, finest rosemary oil 0.52, lavender oil 0.7, orange-blossom water
and rose water each 1.58 quarts, distilled water 2.11 quarts. Proceed
in the same manner as given for qualities I and II.
_Cologne water, quality IV._--Bring into a large glass balloon alcohol
free from fusel oil 7.9 gallons, lavender oil 2.64 ozs., Portugal
oil 2.64, petit-grain oil 0.7, rosemary oil 0.52, bergamot oil 3.52,
lemon oil 3.52, distilled water 7.9 quarts. If this quality, after
standing for some weeks, should not become clear, use some magnesia in
filtering, or use less water.
_Cologne water, quality V._--Bring into a glass balloon alcohol free
from fusel oil 7.9 gallons, Portugal oil 0.88 oz., rosemary oil 0.88,
lavender oil, bergamot oil, and lemon oil each 1.76. After standing for
14 days, add 7.9 quarts of distilled water. Proceed in the same manner
as given for quality IV.
_Maiglöckchen Eau de Cologne._--95 to 96 per cent. alcohol of the
finest quality 10.56 quarts, bergamot oil and lemon oil each 3.52 ozs.,
neroli oil 0.7, French extra lavender oil 0.21, rosemary oil 0.14, best
German balm oil 0.7, ylang-ylang oil 0.17, _maiglöckchen_ (lily of the
valley) extract 2.11 pints.
Dissolve the 0.17 oz. of ylang-ylang oil by itself in 0.8 pint of
alcohol of the best quality, and when the solution is entirely clear
add it to the rest in the balloon. After standing for 14 days add
carefully orange-blossom water and rose water each 1.05 pints; shake
thoroughly and let the mixture stand quietly until perfectly clear.
_Various other receipts for Cologne water._--I. Bergamot oil 2 drachms,
oil of lemon 2 drachms, oil of origanum 6 drops, oil of rosemary 20
drops, alcohol 1 pint, orange-flower water 1 oz.
II. Bergamot oil 14 parts, citron oil 34, oil of neroli (petale) 20,
oil of neroli (bigarade) 7, rosemary oil 14, grape spirit 6000.
III. Cologne spirits 3 quarts, oils of rosemary, bergamot, cedrat, and
lemon each 2 drachms, oil of neroli 1 drachm, water (warm) 2 pints;
mix, filter until clear.
IV. Cologne spirits 3 quarts, oil of lemon 5 drachms, oil of bergamot 4
drachms, Portugal oil 3¾ drachms, neroli oil ¾ drachm, petit-grain
oil and rosemary oil each ½ drachm, lavender oil 25 drops, oil of
cloves 6 drops, extract _Pomm. jasmine_ 4 ozs., water (warm) 32 ozs.;
mix.
V. Cologne spirits 1 gallon, rosemary oil ½ oz., lemon oil 1 oz.,
lavender oil 1½ ozs., cinnamon oil 20 drops, warm water 1 quart; mix.
_Eau de Lavande._--For _eau de lavande_, but two receipts are given:
_Eau de vie de Lavande double ambrée_ and _eau de Lavande double_, the
former being a very agreeable perfume for toilet purposes, and is used
as an addition to wash-water as well as to baths and for fumigating. On
account of its balsamic constituents, _eau de Lavande ambrée_ in being
manufactured cannot be mixed with water, as the latter would produce
an emulsion which cannot be removed. _Eau de Lavande double_ is used
for the toilet, in the wash-water, or the bath. It is very popular, its
action upon the skin and nerves being refreshing and stimulating.
_Eau de vie de Lavande double ambrée._--Alcohol of the best quality
5.18 quarts, best quality of lavender oil 3.52 ozs., French rose
geranium oil 0.7, oils of cassia, bergamot, lemon, and French petit
grain each 0.88, Peru balsam 5.29, orris-root tincture 2.11 quarts,
ambergris tincture 5.29 ozs., musk tincture 0.28, storax tincture 8.81,
tolu-balsam tincture 5.29, benzoin tincture 10.58. No water should be
added.
_Eau de Lavande double._--Best quality of alcohol 10.56 quarts, best
lavender oil 8.81 ozs., Portugal oil and bergamot oil each 1.76. After
14 days add 2.11 pints of orange-blossom water.
_Aqua mellis._--Coriander seed 7 lbs., cloves 12 ozs., storax 8 ozs.,
nutmegs (bruised) 8 ozs., lemon-peel 10 ozs., calamus 6 ozs., proof
spirit 15 pints, water 8 pints.
Macerate for a month in a closed vessel, then distil 22 pints, and to
the distillate add: Orange-flower water 5 pints, rose oil 24 drops,
ambergris 1 grain, vanilla 2 ozs. Macerate for 8 days and filter.
_Eau de Lisbonne._--Lemon oil 2¼ ozs., Portugal oil 4½ ozs., rose oil
4¼ drachms, alcohol 5 quarts.
CHAPTER IX.
DRY PERFUMES.
In ancient times dry perfumes were almost exclusively used, but,
independent of fumigating agents, which will be considered later on,
the consumption of dry or solid perfumes is at present a limited
one. Sachet powders (_poudres pour sachets_) are, however, still
manufactured in large quantities. The preparation of solid perfumes
with the assistance of paraffine has been recently commenced, but up
to the present time such perfumes have not become of any importance.
Smelling salts may also be classed among the dry perfumes.
SACHET POWDERS.--Sachet powders (_poudres pour sachets_) are generally
put into silk or satin bags or into ornamental paper envelopes and are
useful for perfuming clothes, drawers, trunks, desks, letter paper, etc.
The incorporation of the powders with bags or envelopes is effected
by dividing them between thin layers of cotton, bringing the cotton
together with the powder in fine tissue paper into the shape of the
respective bag, cushion, etc., and then inclosing them in the bag or
envelope.
A selection of receipts for such powders is here given. Their
manufacture is not difficult; however, the weighing off of the
constituents should be conscientiously done, and in mixing the powders
with the volatile oils, etc., care should be had not to cause any
unnecessary dust and consequent loss of powder. After mixing, the
powder is passed through a sieve.
_Sachet à la rose._--Ground rose leaves, ground rose wood and
pulverized starch each 50 drachms, Turkish rose oil 1½, rose-geranium
oil 2½, oil of cloves 1, bergamot oil 2½, musk tincture 1.
_Sachet à la violette._--Ground orris root 125 drachms, ground lavender
flowers and pulverized starch each 50, liquid orris-root oil[21] 2½,
sandal-wood oil ½, musk tincture 2, extrait violette 25.
[21] The so-called liquid orris-root oil is not pure orris-root oil,
but generally a distillate of orris-root with bergamot oil; there
are, however, also products in which the orris root is distilled with
copaiba balsam oil and cedar oil.
_Héliotrope sachet powder._--Ground lavender flowers 50 drachms,
ground orris root and ground rose leaves each 25, ground benzoin 10,
pulverized starch 50, bergamot oil 10, rose geranium oil 2½, oil
of cloves and musk tincture each 1½, vanilla tincture 12½, extrait
héliotrope 25, oil of bitter almonds 2 drops.
_Ylang-ylang sachet powder._--Ground starch 100 drachms, orris-root
powder 25, ground lavender flowers 12½, ground vitivert root and ground
rose wood each 25, bergamot oil 2½, ylang-ylang oil 1, tinctures of
musk and of cumarin each 1½, extrait ylang-ylang 20.
_Jockey club sachet._--Ground orris root, ground rose leaves and ground
rose wood each 50 drachms, ground lavender flowers 25, African rose
geranium oil 5, oils of Ceylon cinnamon and bergamot each 2½, oils of
cloves and cedar each 1, musk tincture 2½, civet tincture 1, extrait
jockey club 22½.
_Sachet aux millefleurs._--Ground starch 50 drachms, ground orris
root, ground lavender flowers, ground rose wood, and exhausted vanilla
pulverized, each 50 drachms, pulverized cloves 20, bergamot oil and
African geranium oil each 2½, verbena oil 1, tincture of benzoin and
musk root each 5, musk tincture 5.
_Lily of the valley sachet powder._--Pulverized starch 50 drachms,
ground orris root 25, ground lavender flowers and ground rose wood
each 12½, ground vitivert root and ground benzoin each 25, bergamot
oil 5, wintergreen oil 2, ylang-ylang oil and angelica oil each ½,
bitter almond oil 2 drops, storax tincture 5 drachms, musk tincture 1½,
extrait muguet 25.
_Patchouli sachet powder._--Ground patchouli leaves 100, ground rose
leaves and ground lavender flowers, each 25, patchouli oil 2½, oil of
cloves 1, bergamot oil and African geranium oil each 2½.
_Frangipani sachet powder._--Pulverized starch 25 drachms, ground orris
root 75, ground rose leaves 50, ground lavender flowers 25, Portugal
oil 5, petit-grain oil and African geranium oil, 2½, Ceylon cinnamon
oil 1½, musk tincture 2½, civet tincture 1½, tinctures of cumarin and
vitivert each 10.