IMPROVEMENTS IN THE MANUFACTURE OF SULPHATE OF QUININE
Year: 1853

page_text: LETTERS PATENT to Edward Herring, of Southwark, in the County
of Surrey, Manufacturing Chemist, for the Invention of "IMPROVE-
Sealed the 27th January 1854, and dated the 28th July 1858.
PROVISIONAL SPECIFICATION left by the said Edward Herring at
the Office of the Commissioners of Patents, with his Petition, on
the 28th July 1853.
I, EDWARD HERRING, of Southwark, in the County of Surrey, Manu-
facturing Chemist, do hereby declare the nature of the said Invention
for "IMPROVEMENTS IN THE MANUFACTURE OF SULPHATE OF QUININE" to be
as follows:-
My improvements relate to the complete extraction of quinine from
Peruvian and other suitable barks without the aid of alcohol.
I first boil the powdered bark in solutions of caustic alkali, then
press the bark, & repeatedly agitate it in a tub of cold water. This
decolourized bark is then boiled in sulphuric acid and water, agitated,
run off, & evaporated. This is repeated a second time. The third &
other boilings may be reserved for succeeding portions of decolourized

page_text: bark. I prefer caustic soda, & to evaporate in a water bath at 120° Fali.
I next seperate the flocculent matter by filtering, and treat with dilute
sulphuric acid until exhausted. The washings are to be neutralized by
excess of caustic alkali, and the salt drained, washed, and pressed.
This product is treated with dilute sulphuricacid, and the thick mass
obtained pressed, washed, and again pressed.
In the second or bleaching process the above salt is subjected to one
or two more crystallizations, the solutions being boiled with pure
animal charcoal. The crystals are to be drained and dried.
In my third process the blood red products of the bark obtained in
the first process are to be treated with muriatic acid. The resulting
alkaloids are evaporated & filtered, and precipitated by excess of
lime, which product is to be filtered, pressed, dried, & powdered.
It is now treated by-benzole, or any solvent of quina not a solvent
of lime. The tinctures are to be mixed with dilute sulphuric acid and
water, and agitated, the water extracting the quina, and may be pre-
cipitated by caustic soda. From the calcareous precipitate treated by
any spirit the crude quina may be obtained by distillation, treated
with sulphuric acid, and crystallized into a mass, then pressed, washed,
and again pressed, and twice recrystallized.
The alkali process affords 80 to 90 p. ct of the required produce,
the remaining 10 to 20 p. e being recovered by my third process;
and I claim,-
The process for extracting quina & manufacturing the sulphate
thereof without the employment of alcohol, as described.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Edward Herring in the Great Seal Patent
Office, on the 27th January 1854.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I,
EDWARD HERRING, of Southwark, in the County of Surrey, Manu-
facturing Chemist, send greeting.
WHEREAS Her most Excellen Majesty Queen Victoria, by Her
Letters Patent, bearing date the Twenty-eighth day of July, in the

page_text: year of our Lord One thousand eight hundred and fifty-three, in the
seventeenth year of Her reign, did, for Herself, Her heirs and suc-
cessors, give and grant unto me, the said Edward Herring, Her special
licence that I, the said Edward Herring, my executors, administra-
tors, and assigns, or such others as I, the said Edward Herring, 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, usc,
exercise, and vend, within the United Kingdom of Great Britain and
Ireland, the Channel Islands, and Isle of Man, an Invention for
." IMPROVEMENTS IN THE MANUFACTURE OF SULPHATE OF QUININE," "pon
the condition (amongst others) that I, the said Edward Herring, by
an instrument in writing under my hand and scal, should particu-
larly 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 Seal Patent Office within six calendar months next
and immediately after the date of the said Letters Patent.
NOW KNOW YE, that T, the said Edward Herring, 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:
My said improvements relate to certain processes for the complete
extraction of quinine from Peruvian bark and other suitable barks in
the form of sulphate of quinine, and without the aid of alcohol.
And for the better understanding of my said improvements I will
now proceed to describe my processes in <letail.
In my first process the bark in a powdered state is boiled in a solu-
tion of caustic soda or other alkali, which removes the useless ex-
tractive and gummy colouring matters. After well boiling the bark, it
is to be pressed and returned to a tub to be therein agitated with cold
water, which operation is repeated until the colouring matter is
exhausted. I next proceed to other boilings as follows: in the first
boiling the decolourized bark, after the foregoing process, is boiled in
sulphuric acid and water in due proportions, and kept agitated by suit-
able mechanical means, and this hot solution of sulphate of quinine is

page_text: then run off into an evaporating pan, as customary; the remaining
bark is now boiled a second time in weak sulphuric acid and water, and
run off' as before. The bark may be boiled a third time, or oftener, in
sulphuric acid and water, but as each time the liquid will be less
charged with the sulphates these after boilings may be reserved for
ench succeeding portion of fresh bark decolourized by the first or
alkaline process.
I would here observe that in my first process I prefer using caustic
soda, and that the first and second acid boilings are to be mixed and
evaporated at a temperature of one hundred and twenty degrees
Fahrenheit or thereabouts in a large water bath until sufficiently con-
centrated, and filtered when cool to seperate the flocculent colouring
which then deposits, and which may be treated with ditute sulphuric
acid until exhausted. The filtered cold solution of the first and second
concentrated boilings before named, and also the washings of the
flocculent colouring, are to be neutralized by excess of caustic alkali,
and the precipitated alkaloid drained, washed, and pressed. This last
product is then treated with dilute sulphuric acid, a gentle heat applied,
and the resulting impure sulphates of quinine, quinidin, and cincho-
nine crystallized into a thick mass, which when cold is to be presse‹l,
washed, and again pressed. The pressed cakes thus obtained are next
to be dissolved in a large quantity of water and crystallized as usual.
These crystals will be sufficiently pure for chemical purposes, and afford
the unbleached or hospital sulphate of quinine.
In the second or bleaching process the foregoing sulphate of quinine
is subjected to one or two further crystallizations to produce the pure
white article of commerce, and for this purpose the solutions are boileıl
with a due admixture of pure animal charcoal to avoid contamination
with the free salts of ordinary animal charcoal. The crystals obtained
are to be drained and dried at a low temperature, when they will form
the snow white article of commerce or the bleached sulphate of
quinine.
In my third process the blood red products of the bark boiled in the
caustic soda solution or other caustic alkaline solutions, as described in
the first process, are to be treated with muriatic acid in excess to retain

page_text: the alkaloids in solution which may have been dissolved by the first
soda or other alkaline boilings and washings. These being mixed are
evaporated and then filtered to separate a quantity of colouring matter;
the filtered solution is then to be precipitated by excess of lime, forming
muriate of lime and muriate of soda or other alkali in solution, while
the alkaloids and free lime are precipitated, and may be washed, filtered,
pressed, dried, and powdered. The calcareous precipitate is then ready
to be treated by benzole, or any solvent of the alkaloids that is not a
solvent of lime. These various tinctures or preparations are treated in
the manner following if by benzole or turpentine or lard the
tinctures or preparations are mixed with cold dilute sulphuric acid and
water, and well agitated, the benzole, turpentine, or lard floats, while
the water charged with the sulphuric acid sinks; the acidulated water
having now extracted the alkaloids from the benzole, turpentine, or
other tinctures or preparations, this acid solution is syphoned off into a
convenient vessel, and is precipitated by caustic soda, and the crude
alkaloids are obtained without the application of heat. And herein the
advantage of my improved process consists, rendering such crystals less
amorphous than they otherwise would be by the customary alcohol
process, which does require heat. If the calcareous precipitate has
been treated by alcohol, ether, naptha, or any spirit solvent, the time-
tures are to be submitted to distillation, and the crude alkaloids will be
thereby obtained, but is subject to the objection before named of the
requisite heat rendering the products more amorphous. The crude
alkaloids obtained by either process are to be treated with dilute sul-
phuric acid by gentle heat, and the impure sulphates crystallized into
a mass. These crystals are then pressed, washed, and again pressed,
and are subjected to two or more crystallizations, in order effectually to
remove all trace of impurity, and the produce will then correspond in
quality, though considerably less in quantity, to that obtained in the first
product by my alkali process.
Having this described the nature of my said Invention, I would
remark, that the sulphate of quinine obtained by the alkali process
forms eighty to ninety per cent. of the required product, according to
the quality of the bark, the remaining ten to twenty per cent. being

page_text: recovered by my third process before described. I would have it under-
stood, that my said processes may be variously modified, and yet in
accordance with the principle of my said Invention; and, also, that I do
not claim the use of spirits of wine or of carbonates of the alkalies as
ordinarily employed, but only when applied as in my third before-
described process, wherein I prefer the alkalies, as in the first process,
being in a caustic state, and benzole or other suitable solvents employed
without heat, as already directed. And I do declare, that what I claim
as my Invention is, namely:-
The peculiar processes of manufacturing the sulphate of quinine
without the employment of alcohol, as described.
In witness whereof, I, the said Edward Herring, have hereunto
set my hand and seal, Twenty-third day of January, in the year
four Lord 1854.
EDWARD HERRING. (L.S.)