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DETERMINATION OF AMMONICAL NITROGEN This procedure covers instructions for Determination of Ammonical Nitrogen in water and wastewater. 3. REFERENCE APHA 4500-B&4500-E by Colorimetric method. 4. PROCEDURE STEPS 5.1 GENERAL The sample is buffered at pH 9.5 with a borate buffer to decrease DISCUSSION : hydrolysis of cyanates and organic nitrogen compounds. It is distilled in to a solution of boric acid when titration method is to be used or into H2SO4 when the colorimetric method is used. The ammonia in the distillate can be determined either calorimetrically by the Neslerrizan method. The choice between the colorimetric and the acidimetric methods depends on the concentration of ammonia. Ammonia in the distillate also can be determined by the ammoniaselective electrode method, using 0.04N H2SO4 to trap the ammonia. 5.2APPARATUS : Distillation Apparatus : Arrange a borosilicate glass flask of 500 ml capacity attached to a vertical condenser so that the outlet tip may be submerged below the surface of the receiving acid solution. Use an all borosilicate-glass apparatus or one with condensing units tin or aluminium tubes. PH Meter 5.3 REAGENTS : Distilled water Borate buffer solution: Add 88 ml 0.1N NaOH solution to 500 ml approximately 0.025 M sodium tetra borate (Na2B4O7) solution (9.5 g Na2B4O7.10H2O) and dilute to 1 lit. Sodium hydroxide 6 N De-chlorinating agent: Dissolve 3.5 g sodium thiosulfate (Na2S2O3.5H2O) in water and dilute to 1 L. Prepare fresh weekly. Use 1 L reagent to remove 1 mg/L residual chlorine in 500 ml sample. Neutralisation agent 1) Sodium hydroxide, NaOH, 1N. 2)Sulphuric acid, H2SO4, 1N Absorbent solution, plain boric acid: Dissolve 20 g H3BO3 in water and dilute to 1 lit. Mixed Indicator solution: Dissolve 200mg methyl red indicator in 100 ml 95% ethyl alcohol. Dissolve 100 mg methylene blue in 50 ml 95 % ethyl alcohol and mix both the solution. Indicating boric acid solution: Dissolve 20 g H3BO3 in water and add 10 ml mixed indicator solution and dilute to 1 lit. Preparation of equipment : Add 250 ml water and 10 ml of borate buffer to a distillation flask and adjust pH 9.5 with 6.5 N NaOH solution. Add a few glass beads or -1-

5.4 PROCEDURE:

boiling chips and use this mixture to steam out the distillation apparatus until distillate shows no traces of ammonia. Sample preparation : Use 250 ml de-chlorinated sample or a portion diluted to 250 ml with water. When NH3-N Concentration is less than 100 g/l, use sample volume of 1000 ml, Remove residual chlorine by adding, at the time of collection, dechlorinating agent equivalent to the chlorine residual If necessary, neutralize to approximately pH 7 with dilute acid or base, using a pH meter. Add 10 ml borate buffer solution and adjust to pH 9.5 with 6N NaOH using pH meter. Distillation : To minimize contamination, leave distillation apparatus assembled after steaming out and until just before starting sample distillation. Disconnect steaming out flask and immediate transfer sample distillation apparatus. Distillate at a rate of 6 to 10 ml/min with the tip of the delivery tube below the surface of acid receiving solution. Collect distillate in a 250 ml beaker containing H2SO4 (0.04 N). Collect at least 200 ml distillate. Lower distillation receiver so that the end of the delivery tube is free of contact with the liquid and continue distillation during the last minute or two to cleanse condenser and delivery tube. Dilute to 250 ml with water. Neutralise distillate with 1 N NaOH solution. Ammonia determination : Determine ammonia by the colorimetric method by using Nesslers regent.

5.5 CALCULATION

mg of ammo. Nitrogen x total volume of x 1000 distillate Collected(ml) Ammonical nitrogen(mg/l) = -----------------------------------------Distillate taken for nesslerization(ml) x sample taken (ml)

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