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Ammonical Nitrogen Testing in waste water

 Purpose:

Todescribe the Laboratory Standard Operating Procedure for measurement of Ammonical Nitrogen of Water and Waste Water samples. 

Scope: 

Applicable to the Laboratory for analysis of water and waste water samples, where measurement of Ammonical Nitrogen is required. 

Responsibility:

Lab Chemist:  Analysis of sample for measurement of Ammonical Nitrogen. 

Technical Manager: Review of Activity

Quality Manager: Implementation and compliance of SOP. 

Procedure:

1) Principle:

The sample is buffered at pH 9.5 with borate buffer to decrease hydrolysis of cyanates and organic nitrogen compounds. It is then distilled into boric acid. The ammonia in the distillate is then determined titrimetrically with standard sulfuric acid or calorimetrically. 



2) Instrument and Equipment:

Pipettes, Conical flask, Nitrogen distillation assembly, Heating Mantle. 

3) Reagents:

• Sodium tetraborate 0.025M: Prepare by dissolving 9.5 g Na2B4O7. 10H2O in distilled water and dilute it to 1L.

• Borate buffer solution: Add 88ml 0.1N NaOH solution to 500ml 0.025M sodium tetraborate (Na2B4O7) solution. 

• 6N Sodium Hydroxide: Prepare by dissolving 240g NaOH in distilled water and dilute it to 1 L. 

• Mixed Indicator Solution: Dissolved 200mg Methyle red indicator to 100ml 95% ethanol or propanol . Dissolved 100 mg methylen blue in  50 ml ethanol or propanol. Combine both the solution. 

• Indicating Boric Acid Solution: Dissolved 20g H3BO3 in water add 10ml mixed indicator solution and dilute it ti 1L.

• Sulfuric Acid 0.1N : Dilute 2.8 ml of concentrate sulfuric acid to 1 L with distilled water and standardize this solution with 0.05 N sodium carbonate. 

• Sulfuric acid 0.02 N :

Prepare by accurately diluting 0.1Nsulfuric acid with distilled water. Standardize with sodium carbonate. 

• Sodium Carbonate Solution 0.05N: Dissolve 2.5 gm dried sodium carbonate in distilled water and dilute it to 1L.

4) Test Method:

Distillation:

Use 250 ml de-chlosinated sample or a portion dilute to 250ml with distilled water. 

If necessary neutralize to approximately pH 7.p with dilute acid or alkali. 

Add 25ml borate buffer. 

Adjust pH tp 9.5 with 6N NaOH. 

Attach the flask to distillation apparatus. 

Distill at a rate of 6 to 10 ml/min with the tip of the delivery tube below the surface of receiving acid solution. 

Collect the distillate in the 500ml Erlenmeyer flask containing 59 ml indicating boric acid solution. 

Carry a blank through all steps of the procedure and apply the necessary corrections to the results. 

Titrate ammonia in distillate with standard 0.02N sulfuric acid titrant until indicatir turns a oake-kavender. 

5) Calculation:

Ammonical Nitrogen (mg/l) = (A-B) x N X 14 x 1000/Sample taken ml

Where A=Vol of sulfuric acid titrated for sample. 

B= Vol of sulfuric acid titrated for blank

N= Normality of sulfuric acid used for titration. 

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