Laboratory Methods of Inorganic Chemistry, 2nd English Ed. 1928

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MERCURY FROM CINNABAR. 25

DESULPHURIZATION OF SULPHIDES BY THE PRE-


CIPITATION PROCESS.



  1. Antimony from Stibnite.
    Sulphides containing lead and antimony are frequently treated metallur-
    gically by the so-called "Precipitation Process." By this is understood the
    fusion of the ore with iron and suitable substances to form a slag, whereby
    the iron serves as a desulphurizing agent. The sulphide of iron formed dis-
    solves in the slag, and the precipitated metals collect at the bottom of the
    furnace.


Place a mixture of 100 g. powdered stibnite, 42 g. iron filings,
10 g. anhydrous sodium sulphate, and 2 g. wood-charcoal powder
in a Hessian crucible and heat in a charcoal furnace. The tem-
perature should not rise high enough to melt the iron sulphide
slag completely, but just sufficiently to soften it; this point is
determined by stirring the fusion with an iron rod. After cool-
ing and breaking the crucible a fused mass of antimony, weigh-
ing about 65 g., is found at the bottom. Test a sample of this
crude antimony qualitatively for the presence of arsenic, copper,
iron, and lead.
Purification I. Mix the finely-powdered, crude antimony with
one-fourth its weight of powdered stibnite and an equal amount of
anhydrous sodium carbonate, and melt over the blast lamp in a por-
celain crucible surrounded with a clay mantle. Yield, 60 to 65 g.
Purification II. To remove arsenic from the antimony puri-
fied according to I, pulverize the metal again, mix it with 4 g.

sodium carbonate and 0.2 g. potassium nitrate, and melt the


mixture in the manner just described. Yield, 50 to 55 g. of pure


antimony. Dependent experiment, No. 88.



  1. Mercury from Cinnabar; Sodium and Ammonium
    Amalgams.


Heat a mixture of 23 g. cinnabar and somewhat more than the


calculated amount of iron filings in a small retort of difncultly-


fusible glass. The mercury distils into a small flask which serves


as receiver. Yield, 16 to 18 g.


Sodium Amalgam. Pour the mercury so obtained into a test


tube and add clean, freshly cut pieces of sodium, about the size


of grains of wheat, waiting each time before adding a fresh piece


until the previous one has reacted; toward the end assist the

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