Scientific American Supplement, No. 810, July 11, 1891Various
Science
Scientific American Supplement, No. 810, July 11, 1891
Various
Science -- Periodicals
The precipitated sulphide is dissolved in potassium sulphide, and the
resultant solution, after warming with a little hydrogen peroxide to
discolorize any poly-sulphides that may be present, electrolyzed with
a current of 1.5-2 c.c. of electrolytic gas per minute (10.436 c.c. at
0 deg. and 760 mm. = 1 ampere), when the antimony is deposited as metal
upon the negative electrode. One part of antimony (as metal) in
1,500,000 parts of solution may be thus detected, a reaction thirty
times more delicate than the deposition by means of zinc and
potassium. The stain on the cathode, which latter is best used in the
form of a piece of platinum foil about 1 sq. cm. in diameter, is
distinct even with a solution containing 1/28 mgrm. of antimony; and
by carefully evaporating a little ammonium sulphide on the foil, or
by dissolving the stain in hot hydrochloric acid and then passing a
few bubbles of sulphureted hydrogen gas into the solution, the orange
colored sulphide is obtained as a satisfactory confirmatory test. The
detection of 0.0001 grm. of metal can be fully relied on under all
conditions, and one hour is sufficient to completely precipitate such
small quantities.
_Mercury_.--Mercury is best separated from its nitric acid solution on
a small closely wound spiral of platinum wire. The solution to be
tested is acidified with nitric acid and electrolyzed with a current
of 4-5 c.c. (c.c. refer to c.c. of electrolytic gas per minute). The
deposition is effected in half an hour. The deposited metal is removed
from the spiral by heating the latter gently in a test tube, when the
mercury forms in characteristic globules on the upper portion of the
tube. As a confirmatory and very characteristic test, a crystal of
iodine is dropped into the tube, and the whole allowed to stand for a
short time, when the presence of mercury is indicated by the formation
of the red iodide. 0.0001 grm. of mercury in 150 c.c. of solution can
be clearly detected.
Wolff has applied this test under similar conditions, using a special
form of apparatus and a silver-coated iron anode (this Journal, 1888,
454).
_Lead_.--Lead is precipitated either as PbO_{2} at the anode from a
nitric acid solution or as metal at the cathode from an ammonium
oxalate solution. In both cases a current of 2-3 c.c. suffices to
effect the deposition in one hour.
Here, again, 0.0001 grm. of metal in 150 c.c. of solution can be
easily detected. With both solutions this amount gives a distinct
discoloration to the platinum spiral, on which the deposition is best
effected. As a confirmatory test the deposited metal is dissolved in
nitric acid and tested with sulphureted hydrogen, or the spiral may be
placed in a test tube and warmed with a crystal of iodine, when the
yellow iodide is formed. This latter reaction is very distinct,
especially in the case of the peroxide.
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