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Calcium Oxalate Precipitation Process

Calcium oxalate is precipitated from a hot hydrochloric acid solution treated with ammonium oxalate and neutralized with ammonia. Calcium oxalate has low solubility that decreases further in ammonium oxalate solutions due to the common ion effect. Heating calcium oxalate with sulfuric acid yields coarse crystals suitable for filtration between 70-80°C. Calcium and its alloys are used in metallurgy to deoxidize, degas, desulfurize steel and control inclusions. Calcium removes bismuth as an insoluble compound in lead refining and acts as a reducing agent for less common metals. Calcium is also used in thermal batteries and aluminum

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224 views2 pages

Calcium Oxalate Precipitation Process

Calcium oxalate is precipitated from a hot hydrochloric acid solution treated with ammonium oxalate and neutralized with ammonia. Calcium oxalate has low solubility that decreases further in ammonium oxalate solutions due to the common ion effect. Heating calcium oxalate with sulfuric acid yields coarse crystals suitable for filtration between 70-80°C. Calcium and its alloys are used in metallurgy to deoxidize, degas, desulfurize steel and control inclusions. Calcium removes bismuth as an insoluble compound in lead refining and acts as a reducing agent for less common metals. Calcium is also used in thermal batteries and aluminum

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Hassan Haider
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© Attribution Non-Commercial (BY-NC)
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March 6, 2013

INORGANIC ASSIGNMENT

Reaction Mechanism
The calcium is precipitated as calcium oxalate CaC2O4.H2O by treating a hot hydrochloric acid solution with ammonium oxalate and slowly neutralizing with aqueous ammonia solution Ca+2 + C2O4-2 + H2O CaC2O4.H2O Calcium oxalate monohydrate has the solubility of 0.0067g/dm3 and 0.0140g/dm3 at 25oC and 950C respectively. The solubility is less in neutral solutions containing moderate concentrations of ammonium oxalate owing to Common Ion Effect, Since a dilute solution of ammonium oxalate is employed as Wash Liquid in gravimetric determination. Calcium oxalate being the salt of a weak acid, its solubility increases with increasing hydrogen ion concentration of the solution because of the removal of the oxalate ions to form hydrogen oxalate ions and oxalic acid. CaC2O4 Ca+2 + C2O4-2

C2O4+2 + H+ HC2O4HC2O4- + H+ H2C2O4 This Common Ion Effect gives precipitates of Calcium Oxalate which dissolved in dilute H2SO4 and the liberated oxalic acid its titrated with standard KMnO4 solution. H2C2O4 + KMnO4 + H2SO4MnSO4 + K2SO4 + CO2 + H2O

Effect of Heating
Anhydrous calcium oxalate appears to be stable between 225oC and 398oC. However by water free calcium oxalate along with H2SO4 will give satisfactory result at about 70-80oC. At this temperature coarse crystals are obtained. Precipitation from cold neutral or ammoniacal solutions yields a very finely divided precipitate, which is difficult to filter. Good results are obtained by adding ammonium oxalate to a hot acid solution of calcium salt (more or less calcium oxalate may precipitate, depending upon the pH of the solution) and finally neutralizing with aqueous ammonia solution. The precipitation after digesting for about half an hour consists of relatively coarse crystals which are readily filtered.

March 6, 2013

INORGANIC ASSIGNMENT

INDUSTRIAL USES OF CALCIUM Metallurgical Industries


Metallurgical industries use large amount of calcium or calcium containing alloys for a variety of purposes. In Ferrous Metallurgy, calcium and certain of its alloys are used extensively as addition agents to deoxidize, degas steel, desulfurize and cast iron to control the type and distribution of non metallic inclusions in steel and to promote a uniform microstructure in gray iron. Because of addition of pure calcium to molten steel, it is difficult due to its reactivity. Using alloys such as calcium-silicon may overcome this problem but introduces unwanted alloy elements into the iron or steel. In a new and promising technique a steel-clad calcium wire is quickly fed into molten steel.

Lead Industry
Calcium is used in the lead industry as Refining Agent and as an alloying ingredient. When added to molten lead during refining, calcium metal removes bismuth impurities through formation of the insoluble intermetallic compound Bi2Ca3

As a Reducing Agent
Calcium metal is an excellent Reducing Agent for production of the less common metals because of the large free energy of its oxides and halides For same processes, calcium metal first reacts with hydrogen to form calcium hydride which is then used as the actual reducing agent. Additional amounts of calcium metal are converted into calcium hydride for use as a portable source of hydrogen gas.

In Thermal Batteries

Calcium metal is also used in strip form as the anode material in Thermal Batteries, which are used as the Power Source in artillery fuses.

In Automobile Industry

The mechanical and electrical properties of aluminum alloys are improved through addition of small amounts of calcium. Such calcium containing alloys are used for die casting of automobile trim.

REFERENCES
Vogels (Quantitative Analysis) Encyclopedia Ferman Inorganic Analysis 2

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