Estimation of Ammonia by Titration

PRINCIPLE
111
When sample contains more than 2 mgIL of ammonia-N, as in the case with
domestic sewage and many industrial wastes, the concentration can be determined
by titration with a standard solution of H2S04 after distillation and absorption of
ammonia in boric acid solution.
SELECTION OF SAMPLE SIZE
The Table 3.12 is useful in selecting sample volume for the distillation followed
by titration method.
Table 3.12:
Selection of sample volume for ammonia estimation.
Ammonia-N in sample. mg/L
5-10
10-20
20-50
50-100
APPARATUS
Kjeldahl distillation assembly (Fig. 3.20).
CHEMICALS AND REAGENTS
1. Sodium tetraborate
2. Sodium thiosulfate, Na2Sp3.5Hp
3. Ethyl alcohol
4. Boric acid, H3B03
5. Sodium carbonate, Na2C03
6. Sodium hydroxide, NaOH
7. Methyl red indicator
8. Methyl.blue
9. H2S04
Reagents
Sample volume. mL
250
100
50
25
1. Use ammonia-free water in making all reagents and dilution: This should be
prepared for each batch of samples.
Distillation to prepare ammoniafree water: To each lL of tap water add 2mL
ofa solution of ferrous sulfate (100 gIL FeS04.7HP) and sufficient H2S04 to a
slight acid reaction to methyl orange. Distil with care. Reject the fIrst 50 mL of
distillate and then proceed until three-quarters of the volume of water has distilled
over. Test the absence of ammonia in the distillate with Nessler's reagent.
2. Borate buffer solution: Add 88 mL 0.1 N NaOH (4g1L) solution to 500 mL
112 Handbook of Methods in Environmental Studies
approximately 0.025M di-sodium tetraborate (NalBp,) solution (9.5g
NalBp,.lO Hp per litre) and dilute to 1000 mL.
3. Sodium hydroxide, 6N : Dissolve 24g ofNaOH and dilute to 100 mL.
4. Mixed indicator solution: Dissolve 200 mg of methyl red indicator in 100 mL
95% ethyl alcohol. Dissolve 100 mg methyle blue in 90 mL 95% ethyl alcohol.
Combine these two solutions. Prepare monthly.
S. Indicator boric acid solution: Dissolve 20 g boric acid in ammonia free distilled
water, add 10 mL mixed indicator solution and dilute to IL. Prepare
monthly.
6. Standard sulfuric acid titrant, O.02N: Prepare O.IN HlS04 by diluting 3mL
conc. HlS04 to 1 L. Dilute appropriate volume ofHlS04 to 1 L to obtained 0.02N
HlS04
• 1 mL of 0.02N HlS04 = 0.28 mg N. Standardise it against standard
0.02 N NalCO) solution
7. Dechlorinating agent: For chlorinated drinking water and effluent samples.
Use 1 mL of either (a or b) of the following reagents to remove 1 mgIL of
residual chlorine in 500 mL sample
a. Sodium thiosulfate: Dissolve 3.5 g NalSPr5HP in water and dilute to 1 L.
Prepare weekly.
b. Sodium sulfite: Dissolve 0.9 g NalSOJ in water and dilute to 1 L. Prepare weekly.
PROCEDURE (Fig. 3.20)
Distillation of NH3
1. Take 100 mL of sample in a 500 mL ofKjeldahl flask and add 20 mL of borate
buffer and adjust pH to 9.0 with 6N NaOH solution. Add a few glass-beads of
boiling chips.
2. The contents is heated on low heat for first 10-30 minutes and raise the heat
thereafter for about an 1 h to released all the residual ammonia.
3. Take 50 mL of boric acid cum indicator solution (pink colour solution) in 500
mL of flask and place it below the condenser of the distillation assembly so that
the lower open end of the condenser is dipped in solution.
4. Collect at least 200 mL of distillate in a flask (Pink solution turns to green due
to absorption of ammonia). It is good, to put a mark at the level of 250 mL in
the flask, so that one could easily know when 200 mL distillate is collected.
5. Remove the flask with distillate. Titrate the distillate with 0.02N HlS0 4, to its
original colour (i.e. green to pink colour indicates the end point of titration).
6. Run a distilled water blank in the same manner.