TEST Document UT/Lab/TM/W/015

METHOD No.
Issue Date 01-04-2009

1. TITLE DETERMINATION OF AMMONICAL NITROGEN

2. SCOPE This procedure covers instructions for Determination of Ammonical
Nitrogen in water and wastewater.
3. REFERENCE APHA 4500-B&4500-E by Colorimetric method.
4. AUTHORITY This procedure is approved by Managing Director. It is issued by
& Management Representative. This procedure is implemented by
RESPONSIBIL Laboratory Department.
ITY

5. 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 ammonia-
selective 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

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 TEST Document UT/Lab/TM/W/015
METHOD No.
Issue Date 01-04-2009

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.

5.4 PROCEDURE: • 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
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 µg/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 Nessler’s
regent.

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 TEST Document UT/Lab/TM/W/015
METHOD No.
Issue Date 01-04-2009

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)

Action by/ Responsibility: Chemist

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