Exp.

7: Phosphate Determination by (Vanadomolybdo phosphoric Acid

colorimetric Method)

Phosphorous occurs in waters and wastewaters almost solely as phosphates. The

forms of phosphates arise from a variety of sources. Some small amounts of
orthophosphate are added to some water supplies during treatment. Larger
amounts may be added when the water is used for laundering or other cleaning.

In dilute orthophosphate solution, ammonium molybdate reacts under acid

conditions to form a heteropoly acid, molybdophosphoric acid. In the presence of
vanadium, yellow vanadomolybdophosphoric acid is formed. The intensity of the
yellow color is proportional to phosphate concentration.

Reagents:

1) Ph.Ph Indicator
2) Conc. HCl 1:1 _conc. 1 HCl: 1dH2O
Or conc. 1 H2SO4:1 dH2O

3) Activated carbon, used only when water is colored

- Dry coal at 80 0C for 1 hour, 0.2g to 50 ml sample

4) Vanadate-molybdate reagent
1-Solution (A)
- Dissolve 25 gram ammonium molybdate (NH4)6Mo7O24.4H2O in 300 ml dH2O
2-Solution (B)
- Dissolve 1.25 gram ammonium metavanadate NH4VO3, by heating to boiling in
300 ml dH2O
- Cool, and then add 330 ml conc.HCl, cool solution B to room temperature
Pour solution (A) into solution (B) mix, dilute to 1liter

5) Standard phosphate solution:

Dissolve 0.2195gm anhydrous KH2PO4/1000ml dH2O→50 ppm-p (stock)
You have to make 20 ppm by taking 40 ml stock/100ml dH2O
Dilute waste water 1:10 or 1:5

Note: P rang mg/l wave length used n.m

1-5 400
2-10 420
4-18 470

Prepare Standards: drinking water 1-10ppm

Waste water 1-20 ppm
Procedure:
1- Adjust PH:
-If pH of sample >10, add 1 drop pp Indicator to 50ml sample
-discharge (remove) the red color with 1+1 HCl before diluting to 100 ml by
dH2O
If pH<10 proceed:
2- Remove samples color (if it is colored only)
-Shake about 50ml sample with 200 mg activated carbon for 5 minutes
-Filter through filter paper to remove carbon, color
3- a) Place about 50 ml sample and blank in 50 ml volumetric flask the same thing
with standards (1,2,3,4,5ppm)
b) Add 10 ml vanadate-molybdate reagent dilute to the mark (50ml) by dH2O
After 10 minutes or more:
c) For samples, Blank, standards prepared, read at λ =400nm-
Plot a calibration cure "straight line"

Calculation:
From the calibration curve, find the concentration of the unknown sample.