Environmental Engineering Laboratory By: Ngoc Thuan Le
Phosphate (P-PO4-3) - ascorbic method Principle: Ammonium molybdate and potassium antimonyl tartrate react in acid medium with orthophosphate to form a heteropoly acid-phosphomolybdic acid that is reduced to intensely colored molybdenum blue by ascorbic acid. Apparatus Volumetric tubes, incubator, Spectrophotometer. Procedure 1. Place 40ml of sample to volumetric tubes. 2. Add 4ml of solution of 5V (NH4)6Mo7O24 (ammonium molybdate) and 1V C6H8O7 7.2% (ascorbic acid). Bring the volume to 50ml, mixing after addition. 4. Keep at 20-40oC in incubator for 15 minutes 5. Measure color photometrically at 880nm and compare with calibration curve, using distilled water blank. 6. Calibration curve: P-PO4 solution 0.005mg/ml (5mg/L) Concentration range: 0, 1, 2, 4, 6, 8, 10, 15ml 3.
Calculation
Reagents -
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6g of Ammonium molybdate ((NH4)6Mo7O24.4H2O, 1235.86) + 0.24 gr of antimonyl Potassium tartrate 3-hydrate (C8H4K2O12Sb2.3H2O, 667.87) and 300ml of H2O. Then, adding solution of 120ml H2SO4 (2+1) (mean 2V H2SO4+1V H2O) + 5gr ammonium sulfamate (NH4OSO2NH2, 114.12), bring the solution to 500ml with water. Ascorbic 7.2% (w/v): dissolve 7.2 g ascorbic powder in 100ml dW. Working solution: 5V ammonium molybdate solution: 1V ascorbic. This mixture is stable for 4h. Standard solution, dissolve 0.439gr potassium phosphate monobasic (KH2PO4, 136.09) in water to 1000ml (~ 0.1gr P-PO4 /L, 100mg/L, dilute 20 times before using to have sol’s 5mg/L). Solution for confirmation: dilute 25ml of standard solution to 500ml