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
~Determination of Dioxide in a Manganese Ore.~--Weigh up 0.25 to 0.3
gram of the powdered ore; place in a flask, cover with 10 c.c. of
hydrochloric acid, and close the flask with a paraffined cork, and bulbs
(as shown in fig. 60), having previously charged the bulb with 5 grams
of potassium iodide in strong solution. Heat the flask, and boil
cautiously for about fifteen minutes. Wash the contents of the bulbs
into a large beaker, nearly (but not quite) neutralise with dilute
ammonia, and titrate with the standard "hypo."
As an example, 0.2675 gram of pyrolusite was taken, and required 60.3
c.c. of standard "hypo" (100 c.c. equal 1.185 gram iodine, or 0.4042
gram MnO_{2}), which equals 0.2437 gram of the dioxide or 91.1 per cent.
COLORIMETRIC METHOD.
When compounds of manganese free from chlorides are boiled with nitric
acid and dioxide of lead,[87] the manganese is converted into
permanganic acid, which is soluble and tints the solution violet. The
depth of colour depends on the amount of manganese present, and this
should not much exceed 10 milligrams. A quantity of substance containing
not more than this amount of manganese should be boiled for a few
minutes with 25 c.c. of a solution containing 5 c.c. of nitric acid, and
10 or 20 c.c. of dilute sulphuric acid, with 2 or 3 grams of lead
dioxide. Filter through asbestos, wash by decantation with dilute
sulphuric acid, make up with distilled water[88] to a definite bulk, and
take a measured portion for the colorimetric determination.
The standard solution of manganese is made by dissolving 0.1435 gram of
permanganate of potash (KMnO_{4}) in a little water acidulated with
nitric acid, and diluting to 1 litre. One c.c. will contain 0.05
milligram of manganese.
PRACTICAL EXERCISES.
1. What percentage of manganese (Mn) is contained in permanganate of
potash (KMnO_{4})?
2. Ten c.c. of a solution of permanganate of potash is found to oxidise
10 c.c. of an acid solution of ferrous sulphate. The manganese is
determined in the titrated solution by precipitation as dioxide and
titrating. How much of the ferrous solution will be oxidised in the
second titration?
3. What weight of potassium iodide would be just sufficient to absorb
the chlorine evolved by 0.5 gram of pure dioxide of manganese?
4. What weight of iron must be dissolved up so as to have an excess of
0.25 gram after oxidation by 1 gram of pure dioxide?
5. What weight of the brown oxide, Mn_{2}O_{4} will be left on igniting
1 gram of the pure dioxide?
CHROMIUM.
Chromium occurs in nature chiefly as chromite or chrome iron ore
(FeO_{2}Cr_{2}O_{3}, with more or less MgO and Al_{2}O_{3}), which is
the chief ore. It is a constituent of some silicates, and is frequently
met with in very small quantities in iron ores. It occurs as chromate in
crocoisite (PbCrO_{4}), and some other rare minerals.
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