A text-book of assaying : $b for the use of those connected with mines.Beringer, C. (Cornelius)
Science
A text-book of assaying : $b for the use of those connected with mines.
Beringer, C. (Cornelius)
Assaying
The dry assay of nickel (cobalt being at the same time determined) is
based on the formation of a speise which will carry the cobalt, nickel,
copper, and some of the iron of the ore in combination with arsenic. A
speise of this kind, fused and exposed at a red heat to air, first loses
arsenide of iron by oxidation. It is only when the iron has been
oxidised that the arsenide of cobalt begins to be attacked; and when the
removal of the cobalt is complete, the nickel commences to pass into the
slag, the copper being left till last. The changes are rendered evident
by fusion in contact with borax. The process is as follows:--Weigh up 5
grams of the ore, and calcine thoroughly on a roasting dish in the
muffle. Rub up with some anthracite, and re-roast. Mix intimately with
from 3 to 5 grams of metallic arsenic, and heat in a small covered clay
crucible at dull redness in a muffle until no more fumes of arsenic come
off (about 15 minutes). Take out the crucible, and inject a mixture of
20 grams of carbonate of soda, 5 grams of flour, and 2 grams of fused
borax. Place in the wind furnace, and raise the temperature gradually
until the charge is in a state of tranquil fusion. Pour; when cold,
detach the button of speise, and weigh.
Weigh out carefully a portion of about 1 gram of it. Place a shallow
clay dish in the muffle, and heat it to bright redness; then add about
1.5 gram of borax glass wrapped in a piece of tissue paper; when this
has fused, drop the piece of speise into it. Close the muffle until the
speise has melted, which should be almost at once. The arsenide of iron
will oxidise first, and when this has ceased the surface of the button
brightens. Remove it from the muffle, and quench in water as soon as the
button has solidified. The borax should be coloured slightly blue.
Weigh: the loss is the arsenide of iron. Repeat the operation with the
weighed button on another dish, using rather less borax. Continue the
scorification until a film, green when cold, floating on the surface of
the button shows that the nickel is beginning to oxidise. Cool,
separate, and weigh the button as before. The loss is the arsenide of
cobalt.
If copper is absent, the speise is now arsenide of nickel.
The weight of nickel corresponding to the arsenide got is calculated by
multiplying by 0.607; and, similarly, the weight of the cobalt is
ascertained by multiplying the loss in the last scorification by
0.615.[71] It must be remembered that the nickel and cobalt so obtained
are derived from a fraction only of the speise yielded by the ore taken,
so that the results must be multiplied by the weight of the whole of the
speise, and divided by the weight of the fragment used in the
determination. As an example, suppose 5 grams of ore gave 3.3 grams of
speise, and 1.1 gram of this gave 0.8 gram of nickel arsenide. Then--
0.8×0.607 = 0.4856 gram of nickel
0.4856×3.3/1.1 = 1.456 gram of nickel
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