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Refining Process
Generally the metal extracted from its ore contains some impurities such as unreacted oxide ore, other metals, nonmetals etc. Removal of such impurities associated with the isolated crude metal is called refiing process. In this section, let us discuss some of the common refining methods.
Distillation
This method is employed for low boiling volatile metals like zinc (boiling point 1180 K) and mercury (630 K). In this method, the impure metal is heated to evaporate and the vapours are condensed to get pure metal.
Liquation
This method, is employed to remove the impurities with high melting points from metals having relatively low melting points such as tin (Sn; mp = 904 K), lead (Pb; mp = 600 K), mercury (Hg; mp = 234 K), and bismuth (Bi; mp = 545 K). In this process, the crude metal is heated to form fusible liquid and allowed to flow on a sloping surface.
The impure metal is placed on sloping hearth of a reverberatory furnace and it is heated just above the melting point of the metal in the absence of air, the molten pure metal flows down and the impurities are left behind. The molten metal is collected and solidified.
Electrolytic Refining:
The crude metal is refined by electrolysis. It is carried out in an electrolytic cell containing aqueous solution of the salts of the metal of interest. The rods of impure metal are used as anode and thin strips of pure metal are used as cathode.
The metal of interest dissolves from the anode, pass into the solution while the same amount of metal ions from the solution will be deposited at the cathode. During electrolysis, the less electropositive impurities in the anode, settle down at the bottom and are removed as anode mud.
Let us understand this process by considering electrolytic refiing of silver as an example.
Cathode: Pure silver
Anode: Impure silver rods
Electrolyte: Acidified aqueous solution of silver nitrate.
When a current is passed through the electrodes the following reactions will take place
Reaction at anode Ag(s) → Ag+ (aq) + 1e–
Reaction at cathode Ag+ (aq) + 1e– → Ag(s)
During electrolysis, at the anode the silver atoms lose electrons and enter the solution. The positively charged silver cations migrate towards the cathode and get discharged by gaining electrons and deposited on the cathode. Other metals such as copper, zinc etc.,can also be refined by this process in a similar manner.
Zone Refining
This method is based on the principles of fractional crystallisation. When an impure metal is melted and allowed to solidify, the impurities will prefer to be in the molten region. i.e. impurities are more soluble in the melt than in the solid state metal.
In this process the impure metal is taken in the form of a rod. One end of the rod is heated using a mobile induction heater which results in melting of the metal on that portion of the rod. When the heater is slowly moved to the other end the pure metal crystallises while the impurities will move on to the adjacent molten zone formed due to the movement of the heater. As the heater moves further away, the molten zone containing impurities also moves along with it.
The process is repeated several times by moving the heater in the same direction again and again to achieve the desired purity level. This process is carried out in an inert gas atmosphere to prevent the oxidation of metals. Elements such as germanium (Ge), silicon (Si) and galium (Ga) that are used as semiconductor are refined using this process.
Vapour Phase Method
In this method, the metal is treated with a suitable reagent which can form a volatile compound with the metal. Then the volatile compound is decomposed to give the pure metal. We can understand this method by considering the following process.
Mond Process for Refining Nickel:
The impure nickel is heated in a stream of carbon monoxide at around 350 K. The nickel reacts with the CO to form a highly volatile nickel tetracarbonyl. The solid impurities are left behind.
Ni (s) + 4 CO (g) → [Ni(CO)4] (g)
On heating the nickel tetracarbonyl around 460 K, the complex decomposes to give pure metal.
[Ni(CO)4] (g) → Ni (s) + 4 CO (g)
Van-Arkel Method for Refining Zirconium/Titanium:
This method is based on the thermal decomposition of metal compounds which lead to the formation of pure metals. Titanium and zirconium can be purified using this method. For example, the impure titanium metal is heated in an evacuated vessel with iodine at a temperature of 550 K to form the volatile titanium tetra iodide. (TiI4). The impurities are left behind, as they do not react with iodine.
The volatile titanium tetraiodide vapour is passed over a tungsten filament at a temperature aroud 1800 K. The titanium tetraiodide is decomposed and pure titanium is deposited on the filament. The iodine is reused.
