PHOSPHATE / ROCK PHOSPHATE
To estimate the citric acid – soluble P content in the dicalcium phosphate / rock phosphate sample.
Principle
The residue of the phosphate fertilizer remaining after leaching with distilled water for water-soluble P estimation is extracted with ammonium citrate and the amount of P in the extract is estimated by the volumetric method.
Reagents
1. 1% ammonium citrate
2. Conc. HNO3
3. Dil. HNO3
4. 0.1619 N HNO3
5. 0.1619 N KOH
6. 20% ammonium molybdate
7. Ammonium nitrate
8. Ammonium hydroxide
9. Phenolphthalein indicator
Procedure
Place the filter paper with the residue after leaching for water-soluble P estimation, in a 500 ml conical flask and loosely stopper it. Add 100 ml of neutral ammonium citrate solution of sp. gravity 1.09 and keep the flask on a thermostat at 65oC for one hour, shaking the flask every 5 minutes. Remove the flask from the thermostat and filter the contents immediately through a rapid filter paper (WhatmanNo.5). Wash the residue on the filter paper with warm water (65oC). Collect the filtrate in a 250 ml volumetric flask and make up the volume with distilled water. Estimate the citrate-soluble P content in 25 ml of the extract by Pemberton method.
Calculations
Weight of fertilizer taken:1 g
Weight of the extract prepared:250 ml
Volume of the extract taken for P estimation:25 ml
Volume of 0.1619 N KOH added to dissolve the precipitate:x ml
Volume of 0.1619 N HNO3 used in back titration:y ml
Volume of 0.1619 N KOH utilized to dissolve the ammonium phosphomolybdate precipitate:x-y = z ml
1 ml of 0.1619 N KOH:0.0005 g of P2O5
z ml of 0.1619 N KOH:0.0005 x z g of P2O5
This is present in 25 ml of aliquot
In 250 ml of the ammonium citrate extract
:
g of P2O5
This is present in 1 g of the fertilizer
In 100 g fertilizer ie., per cent of citric acid soluble P2O5 in the fertilizer
:
g of P2O5
(Note : 0.1 N KOH and 0.1 NHNO3 can also be used instead of 0.1619 N acid and alkali. Then the factor for calculation will be 1 ml of 0.1 N KOH = 0.00039 g of P2O5)