OBJECTIVE

To determine and calculate the concentration of ammoniacal nitrogen in the water sample by
titration method

INTRODUCTION

Ammoniacal nitrogen is one of the ways to determine the pollution in waste water, as the
presence of ammoniacal nitrogen at the surface water often indicate as pollution and it is one
of the components of nitrogen. In this situation, ammonia is one of the sources of nitrogen
that helps giving nutrient to algae and other forms of plant life which increase amount of it
leads to overloading in natural system and polluted the water. Moreover, excessive amount
ammonia in water can cause harm to the fish as it is toxic to the fish because of the free (un-
ionised) form of ammonia and the dissolve oxygen in the water decrease as the nitrification
of ammonia happened follows those reaction:-

NH3 + 2O2 HNO3 + H2O

For this Kjeldahl Method that is done in the experiment, these are the reactions that occur in
this experiment:-
ABSTRACT

Ammoniacal nitrogen concentration can indicate the condition of water whether it is polluted
or not. The method that used in this experiment is Kjeldahl Method, the sample need to be
distilled first the titrated with standard sulfuric acid. The sample in this experiment will be
prepared by putting the sample in the distillation flask and dilute with deionized water.
Borate buffer will be added, the addition of NaOH to make sure the pH is 9.5 and
phenolphthalein indicator added. At the other end of the distillation flask is a flask that
contains 25 mL plain adsorbent solution with a methyl red indicator for the titrimetric
method. After the distillation, the distillate was titrated with sulfuric acid and the end point of
the titration is purple-blue color. Then the concentration of ammoniacal nitrogen is calculated
to determine the concentration of the sample. The concentration of the sample is 113.4 mg/L.
MATERIALS AND METHOD

Sample collection and preservation

1. Containers : Plastic or glass

2. Preservation : Acidify with H2SO4 to pH <2.0 and cool at 4̊C
3. Holding time : 7 days

Apparatus

1. Electrical heating device, adjustable

2. Distillation apparatus
A litre round bottom flask, capacity: 300-500mL (24/29), made of Pyrex glass fitted
with a dropping funnel, multiple adapter, splash head, together with a suitable vertical
condenser and a deliver adapter.

Reagents

1. Borate buffer solution:

88 mL of 0.1 N NaOH solution added to 500 mL of 0.025M sodium tetraborete
(Na2B4O7) solution (5g Na2B4O7 or 9.5g Na2B4O710H2O) and diluted to 1 litre.
2. Sodium hydroxide, 6N NaOH:-
240 mL dissolved in 1 litre ammonia-free distilled water.
3. Absorbent solutions, plain boric acid.
20g H3BO3 dissolved in ammonia-free distilled water and diluted to 1L
4. Mixed methyl red indicator
0.2g of methyl red was dissolved in 1000mLor isopropyl alcohol, 0.10g methylene
blue in 50 mL of ethyl or isopropyl alcohol. The solution was combined.
5. Phenolphthalein indicator
6. Ammonium chloride standard
3.819 g NH4Cl dissolved in 1 litre distilled water.
Neutralization agent

1. Sulfuric acid, 1N
2. Sodium hydroxide, 1N
3. Standard sulfuric acid titrant, 0.02N (equivalent to 0.01M)

Procedure:

Sample preparation

1. 100 mL sample or a portion diluted was added to 100 mL deionized water in

distillation flask.
2. 25 mL of borate buffer added and adjusted the pH to 9.5 with 20 mL of 24% NaOH
by using 3 drops of phenolphthalein.

Distillation

1. A 500 mL conical receiving flask prepared with addition of 25mL of plain absorbent
solution and 3 drops of mixed methyl red indicator added for titrimetric method. The
tip of the delivery tube was ensured is below the surface of the absorbent solution.
The delivery adaptor was fitted to this flask.
2. The content of the distillation flask was boiled briefly for 2.50 minutes until 200 mL
of distillate has been collected in the receiver.
3. Excessive frothing avoided, especially when the mixture begun to boil.
4. The distillate was immediately titrated with the standard sulfuric acid, 0.02N by
taking the end point at the appearance of purple-blue colour (pale lavender).
5. With each batch of determination, a control blank was carried out following the exact
procedure using distilled water instead of sample.
RESULTS AND CALCULATION

Volume H2SO4 before Volume H2SO4 after Volume H2SO4 used

titration (mL) titration (mL) (mL)

Blank 17.0 17.5 0.5

Standard 17.6 37.5 19.9
Blank 19.2 19.3 0.1
Sample 5.2 45.8 40.6

Calculation

Each mL of 0.02 N is equivalent to 280µg N

(A−B)×280
Ammoniacal Nitrogen (mg/L) =
S
A = Volume of standard H2SO4, 0.02 N used in titrating sample, mL.
B = Volume of standard H2SO4, 0.02 N used in titrating blank, mL.
C = Volume of sample used (mL)

Standard
(19.9−0.5)×280
Ammoniacal Nitrogen of standard (mg/L) =
100
= 54.32 mg/L

Sample
(40.6−0.1)×280
Ammoniacal Nitrogen of sample (mg/L) =
100
= 113.4 mg/L
DISCUSSION

Ammoniacal nitrogen is a compound that is very soluble in the water as it reacts with the
water and produced ammonium hydroxide. Ammonia in the natural system comes in various
sources. For example it can come from the agricultural activity such as agricultural
development and fertilizer, the discharge chemical from industries to the water body and also
water from household. The water pollution can happened when a higher amount of
ammoniacal nitrogen in the water and it can affect the water as the water will become
pungent and have an odour problem that affect the consumer.

In this experiment, first, the sample needs to prepare by diluting the sample with deionized
water in the distillation flask. Then the addition borate buffer and NaOH as the NaOH added
to adjust the pH of the solution. Phenolphthalien indicator will be added to the solution. The
sample color is light purple. At the other end of the distillation apparatus, the flask will
contain plain absorbent solution and mixed methyl red indicator.

The solution need to be light green color. If the solution turns purple, it needs to be done
again because contamination happened. The contents were boiled until the distillate collected
about 200mL. Excessive frothing need to be avoid during boiling. After the distillation done,
the distillate is titrate with standard sulfuric acid. The color will change from light green and
at the end the color must be purple-blue color. The volume of sulfuric acid used is recorded.

From the result, we can see the volume used for the blank will be lower than the sample. This
shows that the sample contain ammoniacal nitrogen. The ammoniacal nitrogen can be
calculated by using this formula:-

Each mL of 0.02 N is equivalent to 280µg N

(A−B)×280
Ammoniacal Nitrogen (mg/L) =
S
A = Volume of standard H2SO4, 0.02 N used in titrating sample, mL.
B = Volume of standard H2SO4, 0.02 N used in titrating blank, mL.
C = Volume of sample used (mL)

The ammoniacal nitrogen concentration of the standard is 54.32 mg/L and the sample is
113.4 mg/L. The sample shows a higher concentration of ammoniacal nitrogen which means
the sample is waste water that can cause the increase of algae and plants in the water.
CONCLUSION

As a conclusion, the objective of this experiment is achieved because the concentration of the
ammoniacal nitrogen concentration determined. The concentration of ammoniacal nitrogen
the standard is 54.32 mg/L and sample is 113.4 mg/L which mean the concentration of the
sample is high.

REFERENCES

 ‘Ammonia’ by Indah Water retrieved at 24 May 2019 from

https://www.iwk.com.my/do-you-know/ammonia

 ‘Water Pollution: Everything You Need to Know’ retrieved at 24 May 2019 from
https://www.nrdc.org/stories/water-pollution-everything-you-need-know

 ‘How to measure Ammonia and Organic Nitrogen: Kjeldahl Method’ retrieved at 24

May 2019 from http://indiawrm.org/HP-
1/download/38%20Measurement%20of%20Ammonia%20and%20Organic%20Nitrogen.pdf