Carius method:
Procedure:
A known mass of organic compound (wg) containing phosphorus is heated with fuming HNO3 in a sealed tube where C is converted into CO2 and H to H2O. Phosphorous present in the organic compound is oxidised to phosphoric acid which is precipitated as ammonium phospho molybdate by heating with conc. HNO3 and by adding ammonium molybdate.
H3PO4 + 12(NH4)2MoO4 + 21 HNO3 \(\overset{\Delta}{\rightarrow}\) (NH4)PO4.12 MoO3 + 21 NH4NO3 + 12 H2O
The precipitate of ammonium phospho molybdate is filtered, washed, dried and weighed.
Calculation:
Mass of organic compound = Wg
Mass of ammonium phospho molybdate = x g
Molar mass of ammonium phospho molybdate 1877 g
1877 g of ammonium phospho molybdate contains 31g of phosphorous
x g of ammonium phospho molybdate contain = \(\frac{31}{1877}\times\) x g of phosphorous
% of phosphorous = \(\big(\frac{31}{1877}\times\frac{x}{w}\times100\big)\%\) of phosphorous
In an alternate method, phosphoric acid is precipitated as magnesium-ammonium phosphate by adding magnesia mixture. The ppt. is washed dried and ignited to get magnesium pyrophosphate which is washed, dried and weighed.
Weight of magnesium pyrophosphate = y g
Molar mass of magnesium pyrophosphate = 222 g
222 g of magnesium pyrophosphate contains 62 g of P
y g of magnesium pyrophosphate contain = \(\frac{62}{222}\times\) y g of P
% of phosphorous = \(\big(\frac{31}{1877}\times\frac{y}{w}\times100\big)\%\)