IMPROVEMENTS IN OBTAINING PERFUMES, SCENTS, AND ESSENCES BY DIS- TILLATION UNDER VACCUUM, APPLICABLE ALSO FOR OBTAINING TINCTURES AND EXTRACTS OF VARIOUS KINDS
Year: 1874

page_text: ETTERS PATENT to Marshall Mason Harris, of Rochester Square,
Camden Town, in the County of Middlesex, for the Invention of
"IMPROVEMENTS IN OBTAINING PERFUMES, SCENTS, AND ESSENCES BY DIS-
TILLATION UNDER VACCUUM, APPLICABLE ALSO FOR OBTAINING TINCTURES AND
EXTRACTS OF VARIOUS KINDS."--A communication from abroad by
Frederick Walton Edward Harris and John Oliver, of New York,
United States of America.
ealed the 11th December 1874, and dated the 12th June 1874.
PROVISIONAL SPECIFICATION left by the said Marshall Mason
Harris at the Office of the Commissioners of Patents, with his
Petition, on the 12th June 1874.
I, MARSHALL MASON HARRIS, of Rochester Square, Camden Town,
5 in the County of Middlesex, do hereby declare the nature of the said
Invention for "IMPROVEMENTS IN OBTAINING PERFUMES, SCENTS, AND ESSENCES
BY DISTILLATION UNDER VACUUM, APPLICABLE ALSO FOR OBTAINING TINCTURES AND
EXTRACTS OF VARIOUS KINDS," a communication to me from abroad by
:

page_text: Frederick Walton Edward Harris and John Oliver, of New York,
United States of America, to be as follows:-
My Invention consists, first, in the application of a vacuum to the
distillation of flowers, leaves, barks, roots; and other available sub-
stances where the object is to extract the perfume direct from the flowers
or other substances operated upon. To effect this I proceed as follows:-
I have a still, which I prefer should be made very shallow so as to
expose a large surface for evaporation. I place, say for instance, from
10 to 30 gallons of the finest alcohol, previously rendered perfectly pure,
odourless, and of high proof. Connected to this still is a chamber fitted
with trays or frames, in which is placed as many freshly gathered
flowers or other matters to be distilled as will fill the trays and frames
without compression, so that the spirituous vapor to be passed through
these may do so freely, the trays having wire cloth bottoms on which
the flowers or matters rest. This chamber has a lid or cover so
arranged that it can be easily removed and a frame of flowers or
distillable matters put in. This cover is provided with a ring to make
an absolutely air-tight joint, and a screw fastener to hold the cover
down. When this chamber is filled with flowers or distillable substances
and the cover screwed tight hot water, say for instance, 90 to 100
degrees Fab. is admitted to the casing of the still, and the vacuum pump
being put into action evaporation or volatilization of the alcohol sets in,
and the spirit vapor passing through the flowers or matters in distilla-
tion absorbs the essential oil contained in the scent sacs of the flowers
or other matters under distillation, and it is carried forward to the con-
denser where it is condensed as perfume.
As the pump is liable to throw off into the atmosphere a certain
amount of perfume I cause the air after leaving the condenser to pass
through a chamber filled with cotton, wool, or fleece, which has been
previously saturated with oil of ben which absorbs any perfume
remaining. Or I pass the air through a vessel containing oil of ben.
The oil so perfumed can be used for pomades.
When an extremely delicate perfume is required to be produced, such
as otto of roses, violets, and so forth, I proceed as follows :-I use a
small still, in which I place, say for instance, a gallon of distilled water.
This I heat by admitting water, heated say to 90 degrees Fal. into the
casing of the still, so that a very small quantity of aqueous vapour may

page_text: pass off. This is drawn by the action of the vacuum pump through the
chamber which contains the rose leaves, violets, or other flowers or
matters to be treated.
I have also a still of a larger capacity than the one just described, say
10 to 20 gallons, which is filled with pure and odorless alcohol of high
proof. This still is heated by steam or hot water, the latter preferred.
The action is as follows:-The moisture created by the evaporation of
the water passes through the flowers or other substances and carries the
perfume with it, which is absorbed by the spirit vapor as it enters by
pipe from the larger still, and is condensed in a worm as a spirituous.
extract or perfume. In this arrangement a vessel is used containing oil
of ben or cotton wool saturated with oil of ben to intercept the per-
fumed vapors.
It will be understood from the foregoing statement that the above
Invention is also applicable to the production of essential oils from
seeds, roots, and barks of trees, as well as for the preparation of tinctures
and extracts of other kinds.
Sometimes instead of the foregoing mode of proceeding I adopt the
following: I place in the still by way of man-hole the requisite
quantity of purified and high-proof alcohol, and then replace cover on
man-hole. In the receiver is placed the flower leaves or materials to be
operated upon on shelves and the cover fastened down. I open the
valve of the pipe communicating between still and the receiver and
close tightly the valves in pipes so as to cut off communication between
one still and another, and between the still and pipe which joins the
worm. The proper chamber is filled with oil or needed material, and I
securely fasten down the cover on the man-hole. I set air pump in
motion and create the required vacuum in the portions of the machine in
use. One of the the stills and goose neck and pipe not being used in this
O portion of the process are not placed in connection with vacuum pump,
and consequently will not be under vacuo.
So soon as considered proper I admit live steam from the boiler into
the double bottom of the still, and when vaporization of the alcohol in
the still takes place the vapour, passes through the leaves or other sub-
5 stances on the shelves and up through pipe into the worm where it is con-
densed and flows on through the apparatus, from whence it is drawn off
into a small receiver. When distillation has ceased I stop the air pump,

page_text: admit air into machine, empty contents of boiler, and clean out receiver,
and make ready again for next charge.
When an extremely delicate perfume is required to be produced, such
as otto of roses, violets, and such like, I place the required quantity of dis-
tilled water in small still through the man-hole and securely fasten cover
on man-hole. The required quantity of rose leaves or other matter to
be operated upon is put in the large still through man-hole, then securely
fasten, down the cover of the man-hole, and close the globe valve in the
pipe connecting the large still with another chamber or still. I fill the
last-named chamber (now to be used as a still) with the requisite
quantity of pure and odorless high-proof alcohol and then screw down
the cover by means of a fulcrum. I open the globe valve in the pipe
connected to the large still and also the valve in the goose neck of the
small still. The proper chamber is filled with oil of ben or wool or
other material. I set air pump in motion and create a vacuum in the
cntire apparatus.
At the proper time steam or hot water is admitted into the double
bottoms of the stills and into the jacket round the large still. The
distilled water in the small still is heated just sufficiently to throw off
an aqueous vapour which rises and passes through the goose neck and
enters large still, wherein are the flower leaves or other substances.
The contents of the large still are heated to just sufficient degree and
the vapor rises and passes up pipe into another pipe where it is met
with the vapor from the alcohol in the chamber or still before mentioned,
which is vaporized by steam or water admitted into the jacket. The 1
vapors are condensed in the worm and pass through apparatus, and are
drawn off by faucet in receiving chamber. Distillation ceasing, stop air
pump, admit air into machine, empty contents of boiler and appliances,
clean out, and make ready for next charge.
Of course when the chamber where the leaves or other substances to
be distilled is used as a still instead of as a receiver for flower leaves and
such like the shelves are removed before the alcohol is put in.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Marshall Mason Harris in the Great Seal Patent
Office on the 12th December 1874.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, MARSHALL
MASON HARRIS, of Rochester Square, Camden Town, in the County of
Middlesex, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Twelfth day of June, in the year of our Lord
One thousand cight hundred and seventy-four, in the thirty-seventh
year of Her reign, did, for Herself, Her heirs and successors, give and
grant unto me, the said Marshall Mason Harris, Her special licence
that I, the said Marshall Mason Harris, my executors, administrators,
and assigns, or such others as I, the said Marshall Mason Harris, my
executors, administrators, and assigns, should at any time agree with,
and no others, from time to time and at all times thereafter during the
term therein expressed, should and lawfully might make, use, exercise,
and vend, within the United Kingdom of Great Britain and Ireland,
the Channel Islands, and Isle of Man, an Invention for "IMPROVEMENTS
IN OBTAINING Perfumes, Scents, AND ESSENCES BY Distillation under Vacuum,
APPLICABLE ALSO FOR OBTAINING TINCTURES AND EXTRACTS OF VARIOUS KINDS," a
communication to me from abroad by Frederick Walton, Edward Harris,
and John Oliver, of New York, United States of America, upon the
condition (amongst others) that I, the said Marshall Mason Harris, my
executors or administrators, by an instrument in writing under my,
or their, or one of their hands and seals, should particularly describe
and ascertain the nature of the said Invention, and in what manner
the same was to be performed, and cause the same to be filed in the
Great Soal Patent Office within six calendar months next and imme-
diately after the date of the said Letters Patent.
NOW KNOW YE, that I, the said Marshall Mason Harris, do
hereby declare the nature of my said Invention, and in what manner
the same is to be performed, to be particularly described and ascertained
in and by the following statement, reference being had to the Drawings
accompanying these Presents, that is to say:-
In said Drawings Fig. 1 shews one form of apparatus for carrying out
the Invention

page_text: Fig. 2 shews form of apparatus for delicate perfumes.
Fig. 3 shows modified form of apparatus.
My Invention consists, first, in the application of a vacuum to the
distillation of flowers, leaves, barks, roots, and other available substances,
where the object is to extract the perfume direct from the flowers or
other substances operated upon. To effect this I proceed as follows :—
In the still A, Fig. 1, which I prefer should be made very shallow so as
to expose a large surface for evaporation, I place, say for instance, from
ten to thirty gallons of the finest alcohol, previously rendered perfectly
pure, odorless, and of high
proof.
Connected to this still is a
chamber B, Fig. 1, fitted with trays or frames, in which are placed as
many freshly gathered flowers or other matters to be distilled as will fill
the trays and frames a without compressing them, so that the spirituous
vapour to be passed through may do so freely, the trays having wire
cloth bottoms in which the flowers or other matters rest. This chamber
has a lid or cover so arranged that it can be easily removed and a frame
of flowers or distillable matters put in. This cover is provided with a
rubber packing so as to make an absolutely air-tight joint, and a screw
fastener to hold the cover down, as shewn in the Drawings. When
this chamber is filled with flowers, leaves, or distillable substances and
the cover screwed tight, hot water, say for instance 90 to 100 degrees
Fahrenheit, is admitted to the casing d of still A, and the vacuum
pump being put into action evaporation or volatilization of the alcohol
sets in, and the spirit vapour passing through the flowers or matters in
distillation absorbs the essential oil contained in the scent sacs of the
flowers or other matters under distillation, and it is carried forward to
the condenser, where it is condensed as perfume.
As the pump is liable to throw off into the atmosphere a certain
amount of perfume I cause the air after leaving the condenser E to pass
through a chamber H filled with cotton, wool, or fleece, which has been
previously saturated with oil of ben which absorbs any perfume
remaining. Or I pass the air through a vessel containing oil of ben.
The oil so perfumed can be used for pommades and so forth.
When an extremely delicate perfume is required to be produced; such
as otto of roses, violets, and so forth, I proceed as follows:-I use a
· small still A, shewn in Fig. 2, in which I place, say for instance a gallon
of distilled water. This I heat by admitting water heated to, say 90
degrees Fahrenheit, into the casing d of the still, so that a very small

page_text: quantity of aqueous vapour may pass off. This is drawn by the action
of the vacuum pump through the chamber B which contains the rose
leaves, violets, or other flowers or matters to be treated.
I have also a still of larger capacity than the one just described, say
ten to twenty gallons, marked C, which is filled with pure and odourless
alcohol of high proof. This still is heated by steam or hot water, the
latter preferred.
The action is as follows:-The moisture created by the evaporation
of the water passes through the flowers or other substances and carries
the perfume with it, which is absorbed by the spirit vapour as it enters
by pipe at E from still C, and is condensed in the worm D as a spirituous
extract or perfume. In this arrangement I also use a vessel H con-
taining oil of ben or cotton wool saturated with oil of ben to intercept
the perfumed vapours.
My process it will be understood from the foregoing statement is also
applicable to the production of essential oils from seeds, roots, and barks
of trees, as well as for the preparation of tinctures and extracts of other
kinds.
I sometimes instead of the foregoing mode of procedure adopt the
arrangements shown in Fig. 3. In working these arrangements I place
in the still C by way of man-hole n the requisite quantity of purified
and high-proof alcohol and then replace cover on man-hole. In the
receiver D are placed the flowers, leaves, or material to be operated
upon on shelves a in D, and cover is fastened down by means of
fulcrum c, then is opened valve p of the pipe h communicating between
C and D closing tightly the valves p in the pipes i and j, thus cutting
off communication between C and B. and between the still C and the
pipe which joins the worm L. The chamber H is filled with oil or
suitable material, and I securely fasten down the cover on the man-
hole n. I set air pump in motion and create the required vacuum in
the portions of the machine in use, namely in H, G, F, L, k, D, and C.
The still B with goose neck i and pipe j not being used in this portion
of the process are not placed in connection with vacuum pump, and
consequently will not be under vacuo.
So soon as considered proper I admit live steam from the boiler into
the double bottom d of still C, and when vaporization of the alcohol in
the still C takes place the vapor passes into D through the leaves or

page_text: other substances on the shelves a and up through pipe & into tho
worm L where it is condensed and flows into receiver F through the
tube 7, and from F into. G, from whence it is drawn off by the faucet p
in small receiver G. When distillation has ceased I stop the air pump
and admit air into machine, empty contents, and clean out receiver D,
and make ready again for next charge.
.
When an extremely delicate perfume is required to be produced by
the arrangement, Fig. 3, such as otto of roses, violets, and such like, I
place the required quantity of distilled water in small still B through
the man-hole n and securely fasten cover on man-hole. The required
quantity of rose leaves or other matters to be operated upon are put in the
still C through man-hole n, then I securely fasten down the cover of
the man-hole and close the valve p in the pipe & connecting the large
still C with the chamber or still D. I fill the last-named chamber D
(now to be used as a still) with the requisite quantity of pure and
odorless high-proof alcohol and then screw down the cover by means.
of the fulcrum c. I open the valves p in the pipes j connected to tho
large still, also the valve in the goose neck i of the small still B. The
chamber H is filled with oil of ben or wool or other material saturated
with oil of ben, and I set air pump in motion and create a vacuum in
the entire apparatus, namely in H, G, F, L, D, C, and B, the goose
neck and the pipes / and j.
At the proper time steam or hot water is admitted into the double
bottoms d, d, of the stills C and B, and into the jacket K. The distilled
water in the still B is heated just sufficiently to throw off an aqueous
vapour, which rises and passes through the goose neck i and enters C,
wherein are the flowers, leaves, or other substances. The contents of
still C are heated to just sufficient degree and the vapour rises and
passes up the pipe j into another pipe where it is met with the vapour
from the alcohol in the chamber or still D, which is vaporised by steam
or water admitted into the jacket K. The vapours are condensed in the
worm L and pass through the glass tube into receiver F and thence
into G, from whence it is drawn off by faucet p in G. Distillation
ceasing I stop air pump and admit air into machine, I empty contents,.
clean out and make ready for next charge.
Of course when D is being used as a still instead of as a receiver for
flowers, leaves, and so forth, the shelves a, a, a, are removed before the
alcohol is put in.

page_text: In the Drawings the boiler is not shown, but the pipes for connection
to same are shown (marked E). The pipe m, m, Figs. 1, 2, and 3, is in
cach case connected to the air pump which works the apparatus. fare
pipes for outlet of the condensed steam; gare pipes by which to empty
contents of stills; m¹ (Fig. 3), pipes from receiver F and G connected
to chamber H; o represents thermometers; and o¹ is vacuum gauge.
Having now particularly described and ascertained the nature and
object of my Invention and in what manner the same is to be per-
formed or put in practice, I hereby declare that I claim the herein
described Invention of "Improvements in Obtaining Perfumes, Scents,
and Essences by Distillation under Vacuum, Applicable also for
Obtaining Tinctures and Extracts of Various Kinds," as berein-before
set forth and described, it being understood that I do not limit myself
to the precise proportions (or to the details of construction shown in tho
Drawings accompanying these Presents) and) herein described with
reference thereto, as I claim the right to vary such proportions and
details so long as the substantial character of my Invention is pre-
served.
In witness whereof, I, the said Marshall Mason Harris, have
hereunto set my hand and scal, this Twelfth day of December,
in the year of our Lord One thousand eight hundred and seventy-
four.
Witness,
MARSHALL M. HARRIS. (L.s.)
T. MORGAN,
Secretary,
Inventors' Patent Right Association, Limited,
21, Cockspur Street, S.W.