IMPROVEMENTS IN THE PREPARATION OF TETRACHLORIDE OF CARBON
Year: 1866

page_text: LETTERS PATENT to Charles Crump, of Yealmpton, in the County of
Devon, for the Invention of "IMPROVEMENTS IN THE PREPARATION
OF TETRACHLORIDE OF CARBON."
Sealed the 9th July 1866, and dated the 11th January 1866.
PROVISIONAL SPECIFICATION left by the said Charles Crump at the
Office of the Commissioners of Patents, with his Petition, on the
11th January 1866.
I, CHARLES CRUMP, of Yealmpton, in the County of Devon, do hereby
declare the nature of the said Invention for "IMPROVEMENTS IN THE PRE-
PARATION OF TETRACHLORIDE OF CARBON," to be as follows:-
In order to prepare tetrachloride of carbon in accordance with this
Invention iodine is dissolved in bisulphide of carbon contained in a retort
or other suitable vessel, the same being kept cool by being surrounded
with water. Dry chlorine gas is then passed into the liquid so prepared as
long as it is taken up or absorbed thereby, or until crystals of chloride of
iodine appear in the retort. The compound thus formed consists of a
mixture of tetrachloride of carbon and chloride of sulphur, the former of
which may then be partially separated by distillation and the distillate

page_text: purified by treatment with water or milk of lime or potash ley, or in any
other suitable manner as well known to and understood by persons con-
versant with such matters. A very small quantity of iodine is sufficient
for the decomposition of an unlimited amount of bisulphide of carbon,
and instead of using iodine for the purposes of this Invention bromine may
be employed.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Charles Crump in the Great Seal Patent Office on
the 11th July 1866.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, CHARLES
CRUMP, formerly of Yealmpton, in the County of Devon, but now of
Southcombe, Paignton, in the said County, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Eleventh day of January, in the year of our
Lord One thousand eight hundred and sixty-six, in the twenty-ninth year of
Her reign, did, for Herself, Her heirs and successors, give and grant unto
me, the said Charles Crump, Her special licence that I, the said Charles
Crump, my executors, administrators, and assigns, or such others as
I, the said Charles Crump, 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 THE PREPARATION OF TETRACHLORIDE OF CARBON," upon
the condition (amongst others) that I, the said Charles Crump, my
executors or administrators, by an instrument in writing under my, or
their, or one of their hands and seals, should particularly describe anil
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 I, the said Charles Crump, 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, that is to say :-

page_text: My said Invention consists in certain improved processes whereby tetra-
chloride of carbon is more efficiently prepared than by the methods
hitherto employed..
In order to prepare tetrachloride of carbon in accordance with this
Invention I dissolve iodine in bisulphide of carbon, the latter being
contained in a retort or other suitable vessel, and the solution being kept
in a cool state by being surrounded by water or by any other suitable
means. I then pass dry chlorine gas (by the means and in the manner well
known to chemists) into the liquid so prepared as long as it is taken up or
absorbed thereby, or until crystals of chloride of iodine appear in the
retort or other vessel employed. The compound thus formed consists of
a mixture of tetrachloride of carbon and chloride of sulphur, which I then
digest with excess of sulphur in order to convert the higher chlorides of
sulphur which are present into protochloride. The tetrachloride of carbon
is afterwards partially separated by distillation and the distillate purified by
treatment with water or milk of lime or potash ley, or in any other suitable
manner as well known to and understood by persons conversant with such
operations. In some cases, especially when a sufficient amount of chlorine
has not been passed into the solution of iodine in the bisulphide of carbon
as before mentioned, it may be necessary after purifying the tetrachloride
of carbon to complete the purification by dissolving in it a fresh quantity
of iodine and passing in a small additional quantity of chlorine. A very
small quantity of iodine is sufficient to effect the decomposition of an
unlimited amount of bisulphide of carbon, but it will be found desirable
to proportion the quantity of iodine to the rapidity with which the chlorine
is passed into the liquid, so that there shall be enough iodine present to
cause the whole of the chlorine to be absorbed with facility.
I should here mention that bromine may be employed instead of iodine
for the purposes of my said Invention.
Having thus fully declared and ascertained the nature of my said In-
vention, and also the manner in which it is to be performed, I would
observe in conclusion that I do not confine or restrict myself to the precise
particulars of treatment and manipulation of the substances herein-before
mentioned as herein detailed for the purposes aforesaid, inasmuch as varia-
tions may be made therefrom without departing from the main features and
principles of my said Invention; but what I consider novel and original,
and therefore claim as constituting the Invention secured to me by the
said herein-before in part recited Letters Patent is, the preparation of

page_text: tetrachloride of carbon by the action of chloride of iodine or bromine, or
of chlorine in the presence of iodine or bromine dissolved in bisulphide
of carbon, as substantially herein-before set forth and described.
In witness whereof, I, the said Charles Crump, have hereunto
set my hand and seal, this Tenth day of July, in the year of
our Lord One thousand eight hundred and sixty-six.
CHARLES CRUMP. (L.S.)