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Combining submerged membrane technology with anaerobic and ...

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Materials <strong>and</strong> methods2.1.3. Phosphorus compounds2.1.3.1. OrthophosphatesOrthophosphate concentration in wastewater is determined following the method4500-P-E described in St<strong>and</strong>ard Methods for the Examination of Water <strong>and</strong> Wastewater(APHA-AWWA-WPCF, 1998).Ammonium molybdate <strong>and</strong> antimony potassium tartrate react <strong>with</strong> orthophosphate inacid medium to form phosphomolybdic heteropolyacid. This compound is reduced byascorbic acid into molybdate blue.Reagents preparationReagent A: Sulphuric acid 5N.Reagent B: Solution of antimony potassium tartrate. 1.3715 g ofK(SbO)C 4H 4O 6∙0.5H 2O are dissolved in 500 mL of distilled water. This solution must bekept in a bottle <strong>with</strong> glass top in order to be preserved.Reagent C: Solution of ammonium molybdate. 20 g of (NH 4)6Mo 7O 24∙4H 2O aredissolved in 500 mL of distilled water. This solution must be kept in a bottle <strong>with</strong> glass topin order to be preserved.Reagent D: Ascorbic acid 0.01M. This solution is stable for one week.Combined reagent: To prepare 100 mL of the combined reagent, the reagents A to Dare mixed according to the following volumes: 50 mL of reagent A, 5 mL of reagent B, 15mL of reagent C <strong>and</strong> 30 mL of reagent D. The mixture must be stirred after the addition ofeach reagent, following the mentioned order. This combined reagent is stable for 4 hours.Determination procedureA sample of 5 mL is taken <strong>and</strong> one drop of phenolphthalein indicator solution (0.5-1 gphenolphthalein in 1 L of ethanol at 80% concentration) is added. If red color appears,reagent A (H 2SO 4 5N) is added (drops) until the red color disappears. Then, 0.8 mL of thecombined reagent is added <strong>and</strong> the mixture is stirred <strong>with</strong> a vortex stirrer. After 10 minutesbut before 30 minutes, the absorbance at 880 nm is measured <strong>with</strong> a spectrophotometerCecil CE 7200. The quantification is done <strong>with</strong> a 6-8 points calibration curve in the range of0-1 mg P-PO 43-·L -1 , using KH 2PO 4 as st<strong>and</strong>ard (figure 2.6).71

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