THE PHARMACEUTICAL JOURNAL AND TRANSACTIONS. 
[December 7, 1872. 
414 
Tlie London Pharmacopoeia (1851) orders 27 
per cent, more of the alkali than the above, and the 
product is described as “ golden-red.” The Edin¬ 
burgh Pharmacopoeia also orders 27 per cent, more 
of alkali (in this case solution of potash) than the 
B.P. for the preparation of “golden sulpliuret of 
antimony.” The United States Pharmacopoeia 
orders 35 per cent, more alkali (solution of potash) ; 
the product is called “ sulphurated antimony,” and 
is described as a “reddish-brown powder.” In the 
French Pharmacopoeia a totally different process 
is adopted. Sulphide of antimony, flowers of sul¬ 
phur, dried carbonate of sodium, and vegetable 
charcoal are to be heated together in a crucible, and 
when effervescence has ceased, the cooled mass is to 
be exhausted with as little water as possible, the 
solution to be strained off, and precipitated with dilute 
sulphuric acid. The product is Soufre Dore d' Anti- 
moine. 
Experiments .—Having noticed that our laboratory 
students, when working the B.P. process, invariably 
obtained a product of a reddish-brown colour, I 
made a few experiments with a view of ascertaining 
the conditions necessary to the formation of the 
orange-red powder from the B.P. materials, viz., 
black antimony, solution of soda, dilute sulphuric 
acid and water. 
The B.P. process was first tried in its integrity, 
and gave a product of a dark red-brown colour, 
almost maroon, little different in appearance from 
any that had been previously made by the students. 
In the next experiment, one lot of materials was 
boiled hi an open dish, and another lot in a flask; 
otherwise the conditions under which the two ex¬ 
periments were conducted, were precisely similar. 
It was anticipated that, from the greater exposure 
of the materials in the dish, the product obtained 
from them would contain a relatively larger amount 
of oxide than the product of the flask experiment, 
and ‘be correspondingly paler in hue. This was 
found to be the case as regards the colour; the pro¬ 
portion of oxide was not determined. 
Several other experiments, 22 in all, were made, 
in which the B.P. process was modified in various 
ways, so as to include the proportions of materials 
ordered in the Pharmacopoeias referred to above 
except the French, but I failed to obtain a product 
that had the colour mentioned in the Pharmacopoeia. 
The one which most nearly approached the golden 
red of the Pharmacopoeia was got by filtering the 
solution into diluted sulphuric acid. 
In order to compare the dark red product of the 
B.P. process (which I shall call the B.P. product) 
with the sulphurated antimony of commerce, four 
specimens of the latter were procured from well- 
known establishments. The five samples were sub¬ 
mitted to all the B.P. tests except the quantitative one. 
B.P. product .—A red-brown powder, easily mis¬ 
cible with water, and rapidly subsiding from the 
supernatant liquid, which it leaves quite clear. 
Readily acted upon by solution of soda, but does not 
dissolve completely till the mixture is gently warmed, 
when a perfectly clear and colourless solution is ob¬ 
tained. From this solution brilliant crystals are de¬ 
posited after boiling. Readily dissolves in hydro¬ 
chloric acid with evolution of sulphuretted hydro¬ 
gen; the solution is faintly opalescent from the 
separation of a very minute proportion of sulphur. 
After boiling with solution of cream of tartar, the 
filtered liquid gives a slight precipitate with sul¬ 
phuretted hydrogen. Sixty grains treated as the 
Pharmacopoeia directs gave a precipitate of oxy¬ 
chloride weighing 51^ grains. An examination of 
the filtrate showed that a little of the oxychloride 
had washed through. 
No. 1.—(Labelled Antimonium Sulphuratum). An 
orange-red or orange-yellow powder, difficultly 
miscible with water, from which it never subsided 
entirely so as to leave the supernatant liquid quite 
clear. On mixing with solution of soda, a pale buff 
flocculent matter was left undissolved; on boiling, 
the flocks did not dissolve, but appeared to resolve 
themselves into a crystalline powder, and after 
standing for a few hours, brilliant crystals were 
formed on the side of the test tube ; the supernatant 
liquid was bright yellow, evidently from excess of 
sulphur dissolved in the solution of sulphide of so¬ 
dium formed in the decomposition. Partially dis¬ 
solved by hydrochloric acid with evolution of sul¬ 
phuretted hydrogen, and separation of much sulphur 
in flakes coloured bright red,—this colour probably 
due to undissolved sulphide of antimony. After 
boiling with solution of cream of tartar, the filtered 
liquid gave a considerable precipitate with sulphu¬ 
retted hydrogen. 
No. la. — (Labelled Antimonium S ulphuratuni). 
Identical with the preceding in characters and 
reactions. 
No. 2.—A dirty yellowish-brown powder, with pale 
yellow particles plainly discernible in it. Mixes with 
water more readily than No. 1, but not so readily as 
B.P. product. On mixing with solution of soda, very 
dark, almost black flocculent matter was left undis¬ 
solved ; on boiling, the flocks became paler, and 
afterwards the substance behaved like No. 1, which 
it also resembled in its behaviour with hydrochloric 
acid and with solution of cream of tartar and sul¬ 
phuretted hydrogen. 
No. 3.—Similar to No. 1 in appearance, and also 
in its deportment towards the reagents, except that 
the matter insoluble in caustic soda was of a distinct 
red colour, resembling calamine. 
The difference, both in appearance and reactions, 
between the B.P. product and Nos. 1 and la, 
which may be taken as the representatives of 
the trade samples, was so marked that I made 
an attempt to ascertain the composition of each. 
After several experiments, the method finally 
adopted was as follows:—A weighed quantify of 
the sample was heated in the air-bath at 212° 
till it ceased to lose weight; this loss denoted 
hygroscopic moisture. The sample was then digested 
for an hour in a saturated solution of cream of tartar, 
thrown upon a tared filter, washed, dried and 
weighed; this loss was held to denote oxide of an¬ 
timony. A weighed portion of the powder insoluble 
in solution of cream of tartar, was afterwards treated 
with a measured quantity of bisulphide of carbon, 
filtered, and the filtrate evaporated to dryness on the 
water-bath in a tared porcelain dish; the proportion 
of sulphur removed by bisulphide of carbon was 
thus ascertained. What remained after this treat¬ 
ment was presumed to be either the tersulphide of 
of antimony Sb 2 S 3 , or the pentasulphide Sb 2 S 5 . To 
determine which of the two, a weighed quantity of 
the original sample was dropped, a little at a time, 
into a long-necked flask containing fuming nitric 
acid, by which the antimony was oxidized to pentoxide, 
Sb 2 0 5 , and the sulphur to sulphuric acid. The con¬ 
tents of the flask were then washed into a porcelain 
