AN IMPROVED PROCESS FOR PURIFYING OR DISINFECTING ALCOHOL AND ALCOHOLIC LIQUORS
Year: 1869

page_text: LETTERS PATENT to William Edward Newton, of the Office for
Patents, 66, Chancery Lane, in the County of Middlesex, Civil
Engineer, for the Invention of "AN IMPROVED PROCESS FOR PURIFYING
OR DISINFECTING ALCOHOL AND ALCOHOLIC LIQUORS."-A communication
from abroad by Edme Jules Maumené, of Paris, in the Empire of
France.
Sealed the 19th November 1869, and dated the 7th August 1869.
PROVISIONAL SPECIFICATION left by the said William Edward Newton
at the Office of the Commissioners of Patents, with his Petition, on
the 7th August 1869.
I, WILLIAM EDWARD NEWTON, of the Office for Patents, 66, Chancery
Lane, in the County of Middlesex, Civil Engineer, do hereby declare
the nature of the said Invention for "AN IMPROVED PROCESS FOR PURIFYING
OR DISINFECTING ALCOHOL AND ALCOHOLIC LIQUORS," to be as follows:-
The bad taste and smell of some alcohols or alcoholic liquors is due to
the presence of chemical compounds containing sulphur and phosphorus,
A

page_text: and the object of the present Invention is to eliminate these compounds
from the liquor or prevent their formation. To this end I in the first
place dispense with the use of sulphuric acid in the liquid in which the
vegetable substances are fermented, and I employ instead thereof an
equivalent quantity of hydrochloric or other acid not containing sulphur.
The sulphates contained naturally in the fermented substances are
separated therefrom as far as possible by precipitating them by means
of chloride of barium and then separating the baritic precipitate. The
sulphur and phosphorus are eliminated by the use of what may be
termed an alco-metallic substance, as it is a solution of sodium or
potassium in absolute alcohol.
In carrying out the purifying process the alcohol is first treated with
lime, which is allowed to act on it for some time. Then the alco-metallic
solution is added, and a double decomposition takes place when sulphur
and phosphorus compounds are formed, which may be. easily separated,
and the metallic base combines with the alcohol and has neither a dis-
agreeable taste nor smell. The liquor is then distilled in order to free it
from the sulphuret of sodium. A solution of acetate of lead may be
added until no further precipitate is formed, when the clear liquor may
be decanted. It should be understood that potassium or other metals of
that class may be used instead of sodium, the preference given to sodium
being merely on account of the cost. Instead of an alco-metallic
solution pure metals or even alloys of metals may be employed to take
hold of the sulphur.
It will of course be understood that those metals which have the
strongest affinity for sulphur must be employed, such, for instance, as
silver, copper, or lead. The oxides of the metals and other oxides may
also be employed, especially those which part with their oxygen readily,
such as the oxides of silver, mercury, copper, lead, manganese, bismuth,
and antimony. The peroxides are the most suitable for the purpose, and
therefore acid oxides, such as chromic acid and manganic acid, may be
used.
Nitric acid may also be used to give off a portion of its oxygen, for
which purpose it must be added carefully to the alcohol, which must
be kept stirred or agitated.
The bi-chlorides of mercury, silver, lead, or copper, and other chlorides
may also be employed, a preference being given to those of which the
metallic bases combine most readily with sulphur.

page_text: Bromides and iodides may also be employed with advantage. Aqua
regia, which is a mixture of nitric and hydrochloric acids, may also be
employed as an oxidizing agent.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said William Edward Newton in the Great Seal Patent
Office on the 7th February 1870.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, WILLIAM
EDWARD NEWTON, of the Office for Patents, 66, Chancery Lane, in the
County of Middlesex, Civil Engineer, send grecting.
:
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Seventh day of August, in the year of
our Lord One thousand eight hundred and sixty-nine, in the thirty-third
year of Her reign, did, for Herself, Her heirs and successors, give and
grant unto me, the said William Edward Newton, Her special licence
that I, the said William Edward Newton, my executors, administrators,
and assigns, or such others as I, the said William Edward Newton, 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 "AN
IMPROVED PROCESS FOR PURIFYING OR DISINFECTING ALCOHOL AND ALCOHOLIC
LIQUORS," being a communication to me from abroad by Edme Jules
Maumené, of Paris, in the Empire of France, upon the condition
(amongst others) that I, the said William Edward Newton, my exe-
cutors 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 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 William Edward Newton, do hereby
declare the nature of the 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 Drawing here.
2

page_text: unto annexed, and to the letters and figures marked thereon (that is
to say):-
The bad taste and smell of some alcohols or alcoholic liquors are due
to a cause which has not been hitherto ascertained, namely, to the
presence of hydrosulphuric or hydrophosphoric compounds, the least
trace of which may impart to alcohols (properly so called). a very
disagreeable taste. The object of the present Invention is to destroy
these phosphorus or sulphur compounds in a certain and economical
manner. I will first speak of the means of getting rid of the sulphur,
although these. means are, generally speaking, exactly the same for
phosphorus, but it is preferable to describe them as confining their
application to sulphur only, in order to avoid comparisons or repetitions
which would uselessly tire the reader.
All the compounds in question whether of sulphur or phosphorus are
hydrosulphuric ethers, sulphohydrates of organic alkalis, or free hydro-
sulphuric acid, &c., and analogous compounds of phosphorus, in a word,
compounds of sulphur or phosphorus with hydrogen or with compounds
of carbon and hydrogen, or even of carbon, hydrogen, oxygen, azote, &e.,
in which hydrogen predominates and forms with the sulphur or the
phosphorus certain compounds wlrich have a fetid odour, sometimes
extremely so.
Whatever may be the state of the sulphur or phosphorus in these
compounds, the alcohols may be freed from these fetid products by the
following means:- -Firstly, by diminishing as much as possible the
sources of the production of sulphur compounds of all kinds in the
fermentation itself, that is to say, by substituting for the sulphuric
acid which is now added to the liquid, in which beetroot pulps, grain,
potatoes, and other analogous substances are to ferment, its chemical
equivalent of hydrochloric acid or other non-sulphurized acid. The
best developed and most rapid alcoholic fermentation may thus be
obtained without allowing the easy production of the fetid compounds,
as the liquid will only contain the sulphur of the compounds contained
naturally in the fermenting matters, and of which it is almost impossible
to avoid the presence. It is even advisable to separate as much as
possible the sulphur from the natural or accidental sulphates by preci-
pitating these latter previous to fermentation by a suitable dose of
chloride of barium, and the careful separation therefrom of the barytic
deposit. Secondly, by employing for the destruction of the sulphur

page_text: compounds (which render the alcohol impure) one of the methods of
which the following is a general description.
Any means of destroying an organic sulphur compound are good if
they fulfil one at least of the following conditions:-First, the elimi-
nation of the sulphur without substitution (without putting into the
desulphurized molecule another simple body, which is called with greater
or less propriety making a substitution); second, the elimination of
the sulphur by substitution, provided that the substitute be neither
phosphorus, azote, arsenium, antimony, nor silicium; third, to modify
the molecular arrangement without displacing the sulphur, but causing
it to enter into combination with the oxygen and form an acid, which
allows of its being got rid of by alkalis; fourth, to destroy the molecular
arrangement, and cause the sulphur to undergo one of the three
preceding effects.
Moreover these means must be efficacious in alcohol (whether absolute
or not) in phlegms, spirits, and brandies, and also they should not be too
expensive.
These data lead to several distinct modes of operation.
A. Process with Alco-metallic Solutions.-This first method consists
in obtaining absolute alcohol, or at 100° (one hundred hundredths), and
in treating it with a solution, which the inventor calls alco-metallic, that
is to say, a solution of sodium or potassium in absolute alcohol (ethylate
of soda or potash C H³ Na O³, or C H³ K O³,) alcohol at 85° at the
least is produced in the most rapid manner, and in one of the ordinary
apparatus by the usual processes of rectification, but without
any other
object than the most economical production of a concentrated alcohol.
From this primary product we pass to absolute alcohol by adding in the
stills where the last distillation is to take place a quantity of quicklime
in the proportion of at least fifty or sixty kilogrammes per hectolitre,
(sixty if the alcohol is at 85, fifty if it is at 90, &c.) The lime dis-
engages a great deal of heat, and it is advisable to introduce it at several
times, and to take care and maintain the means of condensation, as will
be presently described. The matters are left in contact for twelve hours
at least, and then the distillation is proceeded with, which (this time
without the employment of columns or other ordinary means of
rectification) produces an alcohol which is pure, or at one hundred
hundredths. The alcohol thus obtained will enter into all the most
energetic chemical actions, the reactive agents of which will remain

page_text: inert, or should be employed on a large scale with phlegms in proportion
to the quantity of water mixed with the alcohol. In order to free the
alcohol from the bad taste and smell with which it is still infected a
liquor is now added, which the inventor calls alco-metallic, because it
is formed from alcohol and a metal. Take, for example, a litro of
absolute alcohol and about from fifty to a hundred grammes of metallic
sodium. The alcohol is to be put into a glass flask or into a spherical
receiver with a long neck, and the metal is thrown bit by bit into the
liquid. By slightly heating the receiver in a water bath complete
dissolution of the metal is effected; on cooling the liquid crystals are
sometimes formed, but that does not render the employment of the
liquor more difficult. The solution thus prepared contains the compound
CH³ Na O, that is to say, sodized alcohol or ethylate of soda, the
powerful action of which upon the hydrosulphuric compounds effects
their transformation into products free from sulphur. The unpleasant
taste and smell are thus replaced by an agreeable taste and smell.
The alco-metallic solution is poured into the impure alcohol, while
put in motion more or less rapid by an agitator. In a time, which
is nearly always very short even when cold, the chemical action takes
place, the unpleasant smell and taste disappear as if by magic, and they
are replaced by a smell and taste which are still strong and penetrating,
but aromatic and deprived of all fetidness; this smell and taste will also
somewhat diminish after a time, and in certain cases liquids of an oily
appearance and of a very powerful odour are seen to separate from it,
and may be collected by decantation. These liquids, which possess no
fetidness, are mixtures of divers alcohols C H+ 0% of certain ethers
simple or compound, and other aldehyde products, hydrocarburets, &c.
They are all free from sulphur and have neither in their smell nor tasto
any trace of the fetidness characteristic of impure spirits (esprits du
mauvais goût). These liquids may be sold to manufacturers of chemical
products. The absolute alcohol mixed with the alco-metallic solution
has to undergo a last distillation in order to separate it from the sulphuret
of sodium, soda, and the excess of ethylate of soda employed. Before
submitting it to this operation it is sometimes advisable to add a small
quantity of a second solution or liquor of lead composed of from two to
three hundred grammes of anhydrous acetate of lead dissolved in a litre of
absolute alcohol at 100°. This liquor is to be added (as long as it furnishes
a precipitate) to alcohol treated by the alco-metallic solution; solid sul-
phuret of lead and oxide of lead are formed, which soon deposit, while

page_text: the liquid only contains a small quantity of acetate of soda and plombate
of soda. The deposit is allowed to settle well, the liquid is separated,
and it is submitted to direct distillation (without columns or other'
rectifying apparatus); the alcohol is then pure and of good taste.
This method does not occasion great expense as might be imagined.
The quantity of sodium necessary for disinfecting a hectolitre of alcohol
does not exceed ten grammes in certain cases, and scarcely ever reaches
a hundred grammes. The alco-metallic solution leaves alcohol, which is
added to the mass, and does not occasion any expense. The liquor of
lead costs but little, and the solid residuums, sulphuret of lead, oxide of
lead, and other matters, may be utilized. The lime is not lost, as when
taken from the boilers it may serve for building purposes and the
expense it causes is next to nothing. It will be understood why the
sodium must not be employed direct; the handling of this, metal in
distilling operations, properly so called, would cause continual danger of
fire; these dangers disappear by the employment of the alco-metallic
solution, which is prepared in a detached laboratory, and when once
prepared it cannot in any case cause the ignition of the liquid. The
solution has besides the great advantage of bringing the reagent into
immediate mixture with all parts of the liquid, which ensures at once
the greatest action of the metal upon the sulphur, and a considerable
diminution in the duration of the operations.
Amongst the operations which have just been described the only one
which requires the absence of water in the alcohol, that is to say, requires
the absoluto state of this latter in order to submit it to the chemical
agents, is the reaction of the sodium, or for greater exactness of the
alco-sodic solution, to which water would be an obstacle, not fatal by
any means, as will be seen when speaking of soda, but only in a
pecuniary point of view. The other operations may be effected in
alcohol diluted to from 90° to 85° and even below that; the action of
the alco-sodic liquor itself will not be expensive in many cases for
weak alcohol, and it thus may be very generally employed. I have
only mentioned sodium, but it is evident that potassium and all metals
which will furnish a product of the same order, would act with equal
efficacy; the only reason for the preference given to sodium is its relative
cheapness, and but for this reason potassium or any other analogous metal
might become the base of the liquor.. Products analogous to ethylate
of soda may be obtained with other liquids besides pure alcohol. These

page_text: liquids would however after their action require separation from the
organic radical, which being different from the alcohol would constitute
an impurity. Their use would not therefore be so advantageous, but
their employment is here stated, because in certain cases the result
might be profitable.
Before proceeding further let us consider the apparatus necessary for
the
proper carrying out of the whole process. The fermentation vats do
not undergo any change or addition, and when using hydrochloric acid
all goes on as usual, the only condition necessary is to replace cach
kilogramme of concentrated sulphuric acid (density 1.84) by about
two kilogrammes of hydrochloric acid (density 1.21) according to its
strength.
The second part of the work, viz., the production of a concentrated
alcohol at 85° or ninety hundredths, also does not require novel appa-
ratus. Any of the stills now in use may be conveniently employed to
furnish this alcohol, it is therefore unnecessary to enter into a detailed
description of this part of the operation.
The third part of the operation, viz., the production of absolute
alcohol, may be effected in the ordinary apparatus somewhat modified,
but it is preferable not to adopt these apparatus, which are so useful for
rectifying phlegms, and which would be inconvenient in the present case,
as absolute alcohol is distilled right off and requires no rectification from
the commencement to the end of the work. It is advisable, to operate
in a still composed of, first, a boiler or still; second, a still head with a
froth breaker or anti-primer); third, a refrigerator which gives as little
return as possible into the still.
In the accompanying Drawing, Fig. 1 is a sectional view representing
an arrangement of apparatus which is found to produce good results.
The fourth part of the operation, viz., the addition of the alco-
metallic solution, must be effected out of contact with the air and during
the agitation of the liquid mass. This double condition is fulfilled by
means of the apparatus represented in section at Fig. 2, and which
serves also for adding the lead liquor.
After the operation there is found in the boiler or still a mass of a
more or less grey, greenish, or yellowish color, from which the apparatus
is freed by washing with water; a very alkaline solution is formed, which

page_text: is more or less sulphurous with a deposit of sulphur, lead, &c. All these
products may be disposed of to manufacturers of chemical products.
B. Process by Metals.-The sulphur compounds, the influence of
which has been ascertained, may be destroyed by metals, and the
employment of these bodies becomes in some cases a matter of great
simplicity. We have already seen that sodium or potassium might be
employed direct if those metals (and all those which resemble them) did
not involve great danger of fire. It is much better to employ alco-
metallic solutions than the metals themselves, of which I however claim
the application. Metals which do not furnish alco-metallic solutions
may serve in many cases. For instance, wines contain hydro-sulphuric
products, and are injured by the decomposition of the lye or rather of
the azoted and sulphurous matter which forms the principal part of the
lyes or of the deposits adhering to the sides of casks, vats, and bottles;
the sulphur arising from this source or other analogous ones furnishes
traces of hydro-sulphuric acid; this latter mixes with all parts of the
wine and developes with the "aldehyde" and acetic acid odours which
may be reckoned amongst the most fetid known. A quantity of these
compounds much less than one-tenth of a milligramme in a litre is
sufficient to infect the alcohol. This odour is due to one of the bodies
CHS (sulphurous aldehydes) or Can H 03 S (sulphurous acetio
acids), especially the former. These compounds may be destroyed by the
action of the metals alone, and silver itself may be economically and
advantageously employed for purifying the alcoholic products. For
example, when wine or brandy are in question a thin blade of silver
suspended for a short time in a cask of wine, the fineness of which has
been lost (which is generally due to the cause above mentioned, that is
to say, to the sulphurous products just indicated) will nearly always
suffice to destroy these products; it will be seen to become black, and
will restore to the wine its pristine fineness. This means may be applied
to certain phlegms, and I claim its application to this purpose. All
metals which have an affinity for sulphur may be employed; I have
mentioned the principal ones, viz., silver, copper, and lead, because
they are the most active. These metals are converted into sulphurets
and become consequently black. The sulphurets may be again reduced
to the metallic state at very little expense, which renders the employ-
ment even of silver commercially applicable.
I
It is clear that the metals may be employed in the form of alloys.

page_text: The silver alloy used for coining acts very nearly the same as pure
silver. Alloys of potassium or sodium may in certain cases be advan-
tageously used. I claim the employment for the purposes of the
Invention of metals generally.
C. Process by the Use of Metallic Oxides.-The noxious sulphurous
compounds in question may be destroyed by employing bodies more or
less rich in oxygen, and capable of reacting upon them so as to
transform them into corresponding oxidized products. The sulphur is
separated in nature, or it is itself oxidized so as to remain in solution in
the liquid, but then giving off no longer any fetid odour. One of the
most striking examples is that of oxide of silver prepared by precipi-
tating the solutions of azotate or acetate of silver by an aqueous solution
of potash, soda, or milk of lime (or by other processes). This oxide
will cause the bad odour to disappear from the phlegms with an energy
sometimes surprising, and notwithstanding its high price may produce
very advantageous results.
One fact, however, must be observed, which will be mentioned, and
which establishes a notable distinction between the process by means of
oxides and the following methods. The oxygen of the oxides changes
the sulphurous compounds into oxygenated products, the smell of which
is generally weak, so that this employment in causing the fetidness to
disappear does not replace it by a sharp smell as in the following
methods. The phlegms purified by oxides are flat, but they furnish
alcohol of a pure taste. Many oxides may be employed instead of the
oxide of silver. The most efficacious are those which easily loose their
oxygen; they are well known and are designated in all works on
chemistry. I will however mention the principal ones, the oxides of
silver, mercury, copper, lead, manganese, bismuth, antimony, &c.
peroxides it will be understood are the most active, and for a stronger
reason acid oxides, such as chromic acid, manganic acid, &c., &c. The
oxides are obtained easily, and in two states, anhydrous and hydrated.
The two states are both very favorable to the action in question. This
is clear as regards the hydrates of soda or potash, with regard to which
it is necessary to make a remark of some interest. These hydrates are
casily obtained pure, or to speak correctly without any excess of water
under the formula KOHO. It is sufficient to heat them to redness;
in this state they dissolve in absolute alcohol and constitute a reagent of
great power. Their employment is not in general advantageous for my
The

page_text: object when confining it to this employment only of the alcoholic
solution, but in some cases and often after energetic oxidation of the
sulphur its use is found profitable for neutralizing tho acids on the one
hand, and on
the other for communicating to the alcohol a smell which
is far from being fetid.
According to my general theory an alcoholic solution of potash
contains the compound C H O³ K O, which gives up KO to the acids
and leaves in the alcohol a nascent acid C H O'. The influence of this
acid generates a small quantity of ether of an agreeable odour. Besides
the hydrates, that is to say, the combination of the oxides with water
which is itself an oxide, a number of oxides are known called saline,
because they are formed (like the hydrates) by two oxides, one of which
plays the part of acid and the other that of base. All these oxides may.
be employed with advantage; minium or red oxide of lead is an example
of them; the chromates of potash, of lead, of silver, and the plumbates
of potash and soda or other bases, the stannates of soda, of lime, of lead,
&c., &c., render good service in some cases. I claim the employment
of this class of bodies for the purposes of the Invention.
The limits as above remarked are drawn by particular considerations,
the price in certain cases, the poisonous action in others. Tho rod
oxide of mercury, for example, which is as efficacious as the oxide of
silver in many cases, has no inconveniences in being used for phlegms
intended for distillation, nor for alcohols, but it could not be employed
for wines or brandies.
In a great number of cases the action of the oxides may be aided
by that of other agents, and especially acids. To give one examplo
only, the neutral chromate of potash alone is often almost inefficacious,
but the addition of a certain quantity of hydrochloric acid renders it
very active, and it will then give good results. It will be understood
what variety of resources the series of acids may present without
speaking of the salts and other bodies which will be hercin-after
specially mentioned.
D. Process by the Use of Oxidizing Liquids.--Instead of taking
oxygen from the metallic oxides (free or combined) it may be obtained
from many liquid reagents, the employment of which is more successful
under certain conditions). Azotic (nitric) acid, for example, may be
employed in a profitable manner. The alcoholic mass to be purified

page_text: is put in somewhat rapid motion by means of the agitator shewn in
Fig. 2 of the Drawing, or by any other suitable apparatus, and during
motion a certain quantity of acid is poured in, care being taken to mix
it exactly with all parts of the liquid. In a short space of time, even
in the cold state, the bad smell and taste will disappear and be super-
seded by a sharp and often very agreeable odour. Instead of the
hydrosulphuric compounds, which are so fetid, corresponding oxidised
compounds are produced, and amongst them azotic ethers of a very
penetrating and aromatic odour. This action is produced so much the
better if the alcohol is concentrated as well as the acid.
The operation would be one of the best if there were not some risk of
serious danger. The proportion of concentrated acid (Ac O' HO) to be
employed in a hectolitre of pure alcohol never comes up to half a
kilogramme, and has nothing formidable in itself, but the negligence
or error of a person who should much exceed this quantity would
occasion a danger of explosion or tumultuous upheaving of the liquid
of which it is difficult to control the effects, which might be very
serious. This method may, however, be useful and often effects
the required result with economy, although it necessitates the employ-
ment of non-metallic vessels, and even a special apparatus, represented
at Fig. 3. After having heated the alcohol and acid in this apparatus
a certain quantity of carbonate of soda is added for neutralizing, and
distillation is proceeded with. Many oxidizing solutions may be ranged
under this series, which includes all the liquids having an energetic
oxidizing power. The aqueous or other solutions of manganate of
potash, and of chlorites, hypocharites, &c., &c., oxygenated water, in
a word, all the neutral acid or basic solutions or liquors considered
by chemists as reagents of oxidation. These liquors may be employed
alone or mixed in various proportions according to the kind of alcoholic
liquid to be purified and according to the degree of impurity.
I think it advisable here to describe the special apparatus which I
employ for carrying out the objects described in this Specification.
. In the accompanying Drawing, Fig. 1 represents a vertical section
of the distilling apparatus or condenser. This apparatus consists of
a metal boiler A, serving as a still and containing alcohol up to the
level n, n; P is the man-hole which serves for the supply of lime or
other solid reagents and also for obtaining access for cleaning. In

page_text: the still head B is a perforated diaphragm I for preventing priming;
it is fixed to the sides by brackets, and leaving at its circumference
a space of from five to six millimetres for the passage of the steam.
This anti-primer may be made of finely perforated metal or wire gauze
having meshes of about 2 millimetres in diameter. A second anti-
primer may be placed a little higher if desired. The worm G may
be made of metal or glass; in this latter case it is formed of tubes
connected together by rings of caoutchouc. At the lower extremity of
the worm at H is placed the ordinary apparatus for collecting the alcohol.
The boiler or still, which is provided with all the ordinary accessories,
may be heated by open fire or by steam.
Fig. 2 is a vertical section of the mixing apparatus. A is the
metal boiler, which serves as a still or reacting vessel in which alcohol
is contained up to the level n, n', as shewn by the indicator T, which
serves at the same time for drawing out samples. At the centre of
the boiler is mounted the vertical shaft E, which carries the screw.
beaters m, m', and the metal rods and 1, which may be either plain
or grooved. This shaft is put in motion by bevil gear from the
shaft F, which passes through the stuffing box H, and carries the
fast and loose pullics P, P. The opening Z is brought into com-
munication sometimes with a condenser similar to that represented
at Fig. 1, and sometimes with a column and plate apparatus according
to the arrangement of the operations. I is the man-hole for the
introduction of the reagents and for cleaning, &c. Peepholes S, which
may be round or rectangular, serve to inspect and conduct the operation.
Vis the worm in which the, heating steam circulates; it is fed in at
and escapes at v¹.
Fig. 3 represents another apparatus in longitudinal vertical section.
The boiler A is made of sheet iron lined with lead in order to offer
effectual resistance to all dangerous agents, such as acids or other
reagents capable of acting upon copper. It serves in cases where
the alcoholic liquor to be purified is to be submitted to the action
of the said acids or reagents. The steam for heating the contents
of the boiler circulates in the worm V, and is admitted through the
steam supply cock R. F is the man-hole for cleaning purposes; G is
the steam dome, the orifice E of which is put into communication
with the condenser, Fig. 1, or with the column condensers. Upon
the pipe H are fixed the valves, &c. The level of the alcohol is

page_text: samples.
Process by the Use of Chlorides, Bromides, Iodides, &c.--The sulphur
(or phosphorus) may be removed from fetid alcoholic compounds
and replaced by other bodies besides oxygen. Chlorine, bromine, and
even iodine, &c. may be used to replace it and obtain products nearly
always very agreeable and never fetid. The metallic chlorides M Cl"
generally possess the property of effecting this transformation and
substitution. Their power increases with the number n. According
to this many chlorides may be employed, and not only do they replace
the fetidness from the alcohols but they replace this fetidness by a
sharp penetrating agreeable odour, from which results the advantage
above alluded to for nitric acid of furnishing more aromatic products
than most of the oxygenized products. These products do not occasion
any danger as regards health, as according to the experiments of
Mr. Flourens and others they exert nearly the same action upon the
human body as the natural products which are oxygenized.
One of the most advantageous chlorides to use is the bi-chloride of
mercury, the only inconvenience of which is its poisonous action,
which will perhaps prevent it from being admitted in many manu-
factories. Either alone or in solution in alcohol it acts very energetically
upon the hydrosulphuric products and disinfects alcohols or phlegms
with great rapidity. It is best to employ its alcoholic solution com-
posed as follows:-Pure or aqueous alcohol, one litre bi-chloride, from
one hundred to two hundred grammes. This solution must be
manipulated with the greatest precaution, as any drops thrown into
the eye or coming into contact with the skin or the nails will cause
great danger. The chloride of lead is much less dangerous; it requires
precautions however. Its disinfecting action is very powerful. It may
be employed dry, but it is more prudent to dilute it or dissolve it
first in alcohol. The bi-chloride of tin is very efficacious, and does
not present much danger as a poison.. It may be employed in pure
alcohols or phlegms. For the former it is advisable to cause it to
act in a pure state, for the latter it is preferable to employ it hydrated,
SnCl H O. The handling of the pure chloride would be attended
with great inconveniences; it is a very volatile compound (smoking
liquor of libavius) and its vapors, which are very corrosive, would
injure both the attendants and the apparatus. It is preferable to prepare

page_text: in the laboratory a liquor of tin (or libavius) composed of pure alcohol
one litre, and smoking bi-chloride of tin SnCl2 two hundred and twenty
grammes or thereabouts. This liquor is obtained without much trouble
by surrounding alcohol with ice, or ice and salt, or even simply with
very cold water, and by pouring the chloride in small portions into
the alcohol while in motion; it may be employed almost without injury,
the proportion being at most half a litre for every hectolitre of alcohol.
For weak alcohols or phlegms the crystallized chloride SnCI 5HO may
be employed, or even a solution of chloride in water, alcohol, or the
liquor to be purified. The bi-chloride of copper (32k copper, 35.5
chlorine) is a very powerful agent, but very poisonous. It may be
employed anhydrous brown in alcohol pure or hydrated, either in crystals
or in solution in the weak alcohols, phlegms, &c., which are to be
submitted afterwards to distillation.
It will be seen from these examples that all the chlorides may serve.
The most useful are those the metals of which combine most readily
with sulphur, and this will naturally cause us to fall back upon silver,
copper, lead, mercury, &c.
The chlorides of plantinum and gold notwithstanding their price
may be of service in several cases, as well as all chlorides which easily
part with their chlorine. Bromides and iodides may serve with almost
as much advantage as chlorides, the first, especially, as it is very
rarely that bromine does not produce actions quite similar to those of
chlorine. Bromide of lead acts in the same manner as chloride of
lead, &c. I therefore claim the employment of all these bodies in all
their suitable combinations.
that chlorides combine together or
The numberless compounds which
It is this
It is scarcely necessary to add
with bromides, iodides, oxides, &c.
may be thus obtained often cannot be preferred one before the other,
except by reason of the cost or for other sufficient reason.
especially which prevents a definite choice from being made amongst
even the best of them, and more expressly indicating the same in this
Specification.
F. Process by the Use of Metallic Salts.-There still remains a
branch of compounds, the employment of which is of great utility for
freeing alcohols from their hydrosulphuric products; these are the
salts, and especially the metallic salts, the metals of which combine
most readily with the sulphur. These bodies are most efficacious for

page_text: destroying the fetidness of alcoholic liquids and for replacing this fetid
ness by a very agreeable odour. Amongst the first are to be ranked
the salts of silver, and especially salts with an organic volatile acid, for
instance, acetate of silver. Notwithstanding its high price this salt
will change so completely the smell and taste of alcohol that its em
ployment may be recommended. The silver which it contains unites
with the sulphur, whilst its acid and oxygen give with the organic
radicals of the fetid products an acetic ether or other product mixed
with acetic ether, &c., all bodies which have a very pure and agreeable
odour. The salts of lead or copper may act in the same way, and
without their employment requiring any particular description.
the salts comprised in the definition above given have an action more
or less marked. I therefore claim their employment in all its generality.
The salts may be employed in an anhydrous state for pure alcohol,
for example, or alcohol in solution in water, in weak alcohol, in
phlegms, &c. for effecting the disinfection of these latter. Their action
often takes place under ordinary circumstances of temperature; some-
times it is only properly effected by the application of heat, which is
the case with many insoluble salts.
All
G. Various Processes.-Under this head may be included a certain
number of methods, the results of which are in general less precise or
less advantageous, but which may be serviceable. I therefore wish to
claim them, as it is very possible to improve upon them and to derive
great benefit from them.
Certain agents appear designed to effect with the greatest energy the
destruction of hydrosulphuric compounds, and yet I have not hitherto
mentioned them. Thus it will perhaps seem surprising that chlorine
should not have been found at the head of the reagents indicated in
the foregoing description. But chlorine acts too well, it is difficult
to prevent it from giving rise to the formation of chloride of sulphur,
a compound which, in an excess of alcohol, causes a reproduction of
hydrosulphuric compounds. This is the secret of the well-known failure
of chlorine and its compounds, which act exactly like it. I will now
explain this. Several metallic chlorides have been herein-before men-
tioned the action of which in certain cases is founded upon that of
chlorine, for example bi-chloride of mercury, and it seems that there
is a contradiction therein, but this is only in appearance. For the
purpose of effecting the object of this Invention the bi-chloride is very

page_text: different from chlorine.
Whilst the chlorine which it contains acts
after the manner of free chlorine, its metal prevents the sulphur from
forming chloride of sulphur, and produces sulphuret of mercury, which
escapes entirely from excess of alcohol. Its chlorine, therefore, bears
entirely upon the organic parts of the hydrosulphuric compounds (upon
all which is not sulphur), and forms compounds of good odour, as above
stated. Amongst the reagents which act like chlorine in certain cases,
but otherwise in certain others, aqua regia may be mentioned. This
liquid acts sometimes as a chlorodizer and sometimes as an oxidizer. If
it has not been mentioned amongst the liquid oxidizers it is because
of this double action and to avoid all confusion. Everybody knows
that it is a mixture of hydrochloric acid and nitric acid, and scientific
experience has shewn how its action in its ordinary state must be con-
sidered, but this has not explained what would happen in all possible
cases (that is to say) with a great excess of one acid or the other. I
have examined these extreme cases, and I have ascertained that aqua
regia constituted with a great excess of nitric acid effects the disinfection
of alcohol advantageously. It often produces better effects than this
latter acid employed alone, because it is less exposed to the tumultuous
and fearful actions above mentioned. That which has appeared to be
the best is composed of one kilogramme of ordinary hydrochloric acid
(at 7 or 8 HO) with six to seven kilogrammes of ordinary nitric acid (at
5 or 6 HO). The mixture is made beforehand, and it is introduced
into the alcohol, which may be absolute or only at about 95 90, or
85 hundredths.
In absolute alcohol it is preferable to employ the following solution:
A litre of absolute or pure alcohol, from six to eight litres of absolute.
alcohol containing each about one hundred grammes of fuming nitric
acid. This latter is prepared by adding the acid in small portions to
the alcohol, kept cold by means of well water, ice, or other devices.
The three liquids are mixed in the same manner, with care, in a vessel
surrounded with cold water, and the mixture is used as quickly as
possible without keeping any of it. The action is almost complete in
an instant in alcohol well agitated, or it may be completed by means
of heat if desired. An excess of this reagent must be avoided.
.Second. Certain solutions exercise alone an action which may be
considerably augmented by the addition of other solutions or solid sub-

page_text: stances.
For example, the solutions of chloride of lime (hypochlorite)
and many others already mentioned amongst the liquid oxidizers have
not always by themselves a sufficient action. Some may have been
employed without properly knowing the object to be attained, and have
not been employed under good conditions. They are rendered more
powerful by an addition of acids or other solid or liquid or gaseous
bodies, chosen in such a manner as to produce a suitable chemical
action according to the general principles above set forth. For example,
the solution of chloride of lime has, as is known, much greater activity,
and gives the required result much more rapidly. It is only necessary
to add the acid in quantities insufficient to neutralize the basic oxide,
the potash, or just the equivalent. Then the hydrochloric or other
acid being set free acts as an oxidizer more energetic than the solution
itself without great expence. It will be understood that sulphuric
acid must be avoided as much as possible. Hydrochloric acid will be
the best, avoiding an excess of it, which would cause the mixture to act
as a chloridizer.
Third. There are a great number of bodies which are arrived at
principally in theory, the employment of which is at present somewhat
limited on account of their high price, and which may yet become
profitable. I speak of organic bodies capable of fulfilling the general
condition which serves as the basis of this Invention. It would be
impossible to mention all these bodies without greatly increasing the
length of this Specification, but it will be easy to give general rule
according to which they may be chosen (besides those which are already
included in the preceding paragraphs. This rule is as follows:-Any
body which in presence of a hydrosulphuric compound of organic
nature like itself will separate the sulphur from it and fulfil the con-
ditions indicated in the explanation already given is capable of disin-
fecting alcohols or phlegms, &c., and of imparting a good taste to
them.

page_text: The following is what has been observed upon these two methods of
application-Firstly, it is almost always impossible to be acquainted
with the hydrosulphuric compounds which produce the fetidness of the
alcohols, and consequently it is almost always necessary to attack them
empirically. I will mention several of the bodies the employment of
which has furnished good results in following this course, the chloral
compound C'H CI³ O, the chloric ethers (simple or compound), and
nitric ether. It will be understood that all analogous bodies rich in
chlorine, bromine, iodine, and oxygen will always produce considerable
amelioration at least, and often perfect disinfection and even a develope-
ment of agreeable ethereal odours. I claim therefore the employment of
all these bodies.
Secondly. With a certain number of alcoholic liquids the sulphurous
bodies to which their infection is due may be ascertained. In a like
case it may sometimes be advantageous to determine theoretically the
most suitable substance for obtaining the best reconstitution of the
properly flavored alcohols; I say theoretically or mathematically, because
there now exists a theory according to which the weights may be
calculated of all bodies which take part in a chemical action with the
same precision as has been hitherto calculated. The weight of some of
these matters (for example the weight of an acid) necessary for
saturating an alkali was measured by the equivalents, but when a more
complex action was in question (such as the action of an acid upon
metals for example) there was no exact formula for determining all
the products of that action). This theory is my general theory of
chlorine action. These bases may be resumed in two very simple
formulæ of the same form, the first applicable to actions of contact, the
second to actions of mixture, and comprising in themselves all possible
chemical actions.
To show the utility of these formulæ I will cite two examples, first,
having ascertained that the infection of an alcohol is due to common
hydrosulphuric ether C*H* S, it is required to know what will be the
action of a plate of silver upon this compound if it should be destroyed
and the alcohol disinfected. Silver can only produce one action of contact.
In such a case we have M: M'x ::D mass of the ether or mass of silver,
density of equivalent =45=x, the ether =0.84-D'; density of the silver
10.47, whence x=560 g, that is to say, that the weight of silver which

page_text: 560-9
108
may contribute to the chemical action is 560 grammes 9 when the weight
of ether is 45 gr. (or equivalent). We have afterwards =5.19;-108
is the equivalent of the silver;-the 560 gr ;-9 represents therefore 5.19
equivalents. Now the equivalent of silver is sufficient to destroy the equi-
valent C'H'S, there will therefore remain an excess of silver according
to the formula 5Ag+C HS-CH3 +AgS+4Ag. The ether will be
reduced to C'H', or ethyle which has not a fetid odour, sulphuret of
silver AgS which has no effect on alcohol, and there will remain 4Ag.
In a word, the silver which may be brought into the presence of ether
may, whatever may be its proportion, exert a forcible action, and if a
powerful equivalent be employed will disinfect the alcohol.
99
Second. In the second place it is required to know if another body,
Hollands (C* H* C12) for example, will also produce a good effect. This
liquor dissolved in alcohol will produce a mixing action, and this time
there will be an action by equal weights. The equivalent 99 of the
Dutch liquor will act upon 99 of ether, or =2.2 equivalents, we shall
have then 2 CHS+CH C1-C H+CH+2CIS. The ether and the
liquor are transformed into C8 H (hydruret of tetresü), C* II' (diene), two
bodies which have no fetid odour; 2CIS chloride of sulphur, which in
the excess of alcohol will reproduce hydrosulphuric compounds.
above stated the alcohol will not be disinfected.
As
The calculation is almost always as simple as in the two examples just
given. Sometimes the first action is followed by one or more secondary
actions, which are calculated by applying the same principles without
any particular difficulty. Thus, by applying the theory every time that
the exact nature of the hydrosulphuric compounds is ascertained the
effect may be judged beforehand of what is produced by any reagents
the employment of which might appear commercially applicable (that
is to say) economical. This theory is the only one which allows a
calculation to be made of all the bodies developed in one single action;
the theories hitherto admitted only furnish remarks more or less general,
which may aid in explaining the results of the two fundamental formula
above given.
Any organic or other compound which according to the onc or other
of these laws is capable of transforming hydrosulphuric compounds
into compounds of oxygen, chlorine, bromine, iodine, or even fluorine

page_text: is good for effecting the disinfection of alcohols and reproducing a
proper flavour. The best are those which furnish oxygenous or chlorine
products. Those which give phosphorous, arsenious, antimonious, or
silicious compounds should be thrown aside.
I claim the employment generally of all bodies the use of which has
been herein-before clearly defined.
It will be advisable in conclusion to repeat as regards phosphorus
what I have said at the commencement of this Specification. It is
nearly always eliminated by the same means as sulphur when it requires
a different reagent; this reagent belongs to one of the other methods
above mentioned, there will therefore be a real and industrial solution of
the difficulty.
It may be here desirable to give some details as to the utilization of
the high-priced residues the loss of which should be avoided.
Compounds of mercury, silver, gold, and platinum must not be wasted.
In order to extract them reference might be had to Treatises upon
Chemistry, but I will briefly point out the most simple means.
One of two things must take place, either the reagent employed will
be found in the lyes or analogous residua in an entirely insoluble state,
or it will be partly soluble and partly insoluble. The whole is first to
be rendered insoluble. For this purpose a certain quantity of sulphuret
of sodium (or potassium or calcium) is to be poured in as long as a black
or brown color is produced, it is then stirred and left to settle. The
sediment contains all the precious metal ordinarily all in the state of
sulphuret. It is dried upon cloths and roasted in a refining vessel and
melted at a red heat with carbonate of soda (and one-tenth of saltpetre);
mercury requires other apparatus, which is described in all treatises
upon chemistry. By this means a lump of silver or gold or spongy
platinum is obtained, which may be readily melted down or converted
into a chloride of other product.
The soluble or insoluble silver may be, by preference, collected in the
form of a chloride. For this purpose a little excess of hydrochloric acid
is poured into the residuum (vinasses) and the sediment or precipitate
is treated as in the preceding case; or the sediment or precipitate might

page_text: be disposed of to manufacturers of chemical products, by whom the
reduction of the metals may be effected.
In witness whereof, I, the said William Edward Newton, have here-
unto set my hand and seal, the Seventh day of February, in the
year of our Lord One thousand eight hundred and seventy.