CMT 565

EXPERIMENT 5
LTM : AMMONIACAL NITROGEN
(NH3)
NAME INAS SYUHAIDAH BINTI CHAIRIL ANWAR
STUDENT ID 2017420012
GROUP AS245 4M3C
NAME OF PARTNERS 1. NURUL AFIQAH BINTI MAT AZMAN
2. MUHAMMAD SHUKERI BIN RAZMAN
3. NURFAZA BINTI ZAIMON
DATE OF EXPERIMENT 3/4/2019
DATE OF SUBMISSION 3/05/2019
 EXPERIMENT 5 :
LTM : AMMONIACAL NITROGEN (NH3)

1. OBJECTIVE

To determine the concentration of ammoniacal nitrogen in the waste water sample.

2. INTRODUCTION
Nitrogen is an essential ingredient in the formation of proteins for cell growth.
From complex organisms like animals to the simple bacteria used to treat wastes in an
activated sludge treatment facility. Every living thing needs some form of nitrogen to
survive. Ammonia can be converted to nitrite (NO2) and nitrate (NO3) by bacteria and
then used by plants. Ammonia is excreted by animals and produced during
decomposition of plants and animals thus returning nitrogen to the aquatic system.
Ammonia is also one of the most important pollutants because it can be toxic causing
lower reproduction and growth. The neutral unionized form (NH3 ) is highly toxic to fish
and other aquatic life. Ammonia and nitrogen compounds are applied directly as
fertilizers.

The typical output of liquid manure from a dairy farm after separation from the
solids is 1600 mg/L of NH3-N . Sewage treatment plants receiving lower values,
typically remove 80% and more of input ammonia and reach NH3-N values of 250 mg/L
or less. Excessive ammoniacal nitrogen in waterways can cause taste and pungent odor
problems it will be under the impression that the water source is contaminated with
sewage. Higher concentrations of ammonia that discharged into our water ways can
contribute to eutrophication.

Excessive nitrogen concentration in the environment can lead to changes in the

natural nitrogen cycle between living beings, soil, water and atmosphere. The nitrogen
can causes nitrification. Nitrification is the oxidation of reduced forms of nitrogen
ultimately to nitrate. The nitrification process can have a direct impact on water quality.
The end result of nitrification, nitrate (NO-) is a form of nitrogen that is highly mobile
and easily moves with water.

In this experiment, the nitrogen are determined and measured in wastewater in

different water sampes such as lake water from section 7. It is used as one indicator
of water quality. To measure the water quality, it have parameter limits of standards A
and B by Malaysia Sewage and Industrial Effluent Discharge Standards.
3. LITERATURE REVIEW

The method used to determine the nitrogen in the wastewater was APHA 4500-
NH3 B which is preliminary distillation step. Traces of ammonia was elimated in distilled
water by adding H2SO4 to distilled water and redistilling. The redistilled water was
checked for the possibility of a high blank. It is very difficult to store ammonia-free water
in the laboratory without contamination from gaseous ammonia. If a high blank value is
produced, fresh ammonia-free water was prepared.

Nitrogen (N) pollution has increased remarkably over the past several decades as
a result of increased creation of reactive N for fertilizer used (Galloway et al. 2004).
Nitrogen makes up approximately 78% of the earth’s atmosphere and is the fifth most
abundant element in the universe (Gagnon, 2015). Removal of nitrogenous compounds
needs to be considered in STP design. These compounds found in various forms such as
ammonia or ammoniacal nitrogen, nitrate nitrogen and nitrite nitrogen could be
detrimental to natural water bodies and potable consumption. Total organic nitrogenous
compounds in raw sewage typically comprise of nitrogen in the form of proteins, amino
acids and urea along with ammoniacal nitrogen. High levels of ammonia in aquatic
environments can lead to eutrophication, oxygen depletion, and toxicity to aquatic
animals. An important goal of municipal wastewater treatment plants (WWTPs) is to
remove ammonia from human waste before the treated effluent is released into receiving
waters. High concentrations of ammonia, nitrite and nitrate in an aquatic environment can
also be toxic to animals and especially fish (Comargo and Alonso, 2007).

There are various sources of ammonia in rivers as follows:-

 fertilizers for land and agricultural developments.

 uncontrolled landfill leachate and land development.
 wastewater discharges from domestic, commercial, institutional and similar
facilities.
 wastewater and toxic chemicals discharges from different types of industries
 surface runoff and washouts resulting from rainfall
 oil, sullage (wastewater) from bathrooms and kitchens
 municipal sewage treatment plant effluent
 Ammonia-nitrogenNH3 -N is a constituent in raw domestic wastewater. In December
2009, the Department of Environment (D.O.E) Malaysia has revised the Environmental
Quality (Sewage) Regulations 2009, which significantly reduced the discharge limit of
ammonia-nitrogen from 50 mg/L to 5 mg/L. In addition, a new discharge limit was also set
for nitrate at 10 mg/L.
4. MATERIALS AND APPARATUS

 Heating funnel  Ammonium chloride standard,

 Distillation flasl 1000ppm
 Conical receiving flask  Sulphuric acid, 1N
 Retort stand  Sodium hydroxide, 1N
 Burette  Standard Sulfuric acid titrant, 0.02N
 Borate buffer solution  Mixed methyl red indicator
 Sodium hydroxide, 6N NaOH  Phenolphthalein indicator
 Absorbent solutions, plain boric
acid

5. METHODS
For sample preparation, 100ml sample or a portion diluted to 100ml deionized water was
added in a distillation flask. 25ml of borate buffer was added and pH was adjusted to 9.5
with 20ml of of 24% NaOH using 3 drops of phenolphthalein indicator. For distillation,
500ml conical receiving flask was prepared with additional of 25ml of plain absorbent
solution. 2 to 3 drops of mixed methyl red indicator was added for titrimetric method.
The tip of the delivery tube must below the surface of the absorbent solution. The
delivery adaptor was fitted to this flask. The contents of the distillation flask briskly was
boiled for 2.5 minutes until about 200ml of distillate has been collected in the receiver.
The distillate was titrated immediately with the standard sulphuric acid, 0.02N by taking
the end point at the appearance of a purple-blue colour. For each batch of determination,
carried out a control blank following exactly the same procedure using distilled water
instead of sample.
6. RESULT AND CALCULATION

Volume of Standard Sulphuric Acid

used in titration with distillate (ml)
1st trial 2nd trial
Blank 0.5 0.4
Standard 8.1 8.0
Sample (Section 7) 0.8 0.9

(𝐴−𝐵)× 280
Ammoniacal Nitrogen (mg/L) = 𝑆

A = volume of standard H2SO4, 0.02N used in titrating sample, ml

B = volume of standard H2SO4, 0.02N used in titrating blank, ml
S = volume of sample used (ml)

1st trial 2nd trial

Standard Standard

(8.1−0.5)× 280 (8.0−0.4)× 280

= =
100 100

= 21.28 mg/L = 21.28 mg/L

Sample (Section 7) Sample (Section 7)

(0.8−0.5)× 280 (0.9−0.4)× 280

= =
100 100

= 0.84 mg/L = 1.40 mg/L

 7. DISCUSSIONS

In this experiment, the amount of Total Suspended Solids (TSS) was calculated in water
sample. Water sample that used was distilled water that known as blank, standard that have been
prepared and water from lake section 7. The removal of nitrogen from wastewater has become an
emerging worldwide concern because these compounds cause eutrophication in natural water.
Moreover, nitrate is a risk to human health. The effluent from wastewater treatment plants has
remaining and nitrogen in the form of ammonium and/or nitrate. The forms of nitrogen most
prevalent in waste waters which required treatment. Malaysian government has taken a step to
introduce the N discharge limit in the Environment Quality (Sewage) Regulation 2009. Table 1
details the discharge limits imposed on the new sewage treatment plants. The regulation requires
the plants to meet the effluent P limit of 5.0 mg/l in Standard A and 5.0 mg/l in Standard B
(Department of Environment, Malaysia, 2010).

Table 1: Environment Quality (Sewage) Regulation 2009 for new sewage treatment system.

Parameter Unit Standard A Standard B

Temperature ̊C 40 40
pH value - 6.0-9.0 5.5-9.0
BOD mg/L 20 50
COD mg/L 120 200
Suspended Solids mg/L 50 100
Oil and Grease mg/L 5.0 10.0
Ammoniacal Nitrogen (enclosed water body) mg/L 5.0 5.0
Ammoniacal Nitrogen (river) mg/L 10.0 20.0
Nitrate-nitrogen (enclosed water body) mg/L 10.0 10.0
Nitrate-nitrogen (river) mg/L 20.0 50.0
Phosphorus mg/L 5.0 10.0
Standard A for discharges upstream of water supply intake points or any sensitive areas.
Standard B for discharges downstream of water intake points or any other areas that do not fall
under standard A.
 Based on the result, the average amound of ammoniacal nitrogen in standard was
calculated was 21.28 mg/L. While, the average concentration in water samples from section 7
contains 1.12 mg/L. This ammonia content reading in the sample is lower compared to two
standards for effluent discharge: Standard A and Standard B. Water from the section 7 was
considered effluent. Effluent is an outflowing of water or gas to a natural body of water, from a
structure such as a wastewater treatment plant, sewer pipe or industrial outfall. Water sample
from section 7 was compared with Standard B. This is because Standard B for discharge
downstream of any raw water intake. The Standard B shows that the value for ammoniacal
nitrogen was 5 mg/L. The result is in the range. Based on the result in table 2 from the other
group, the amount of ammoniacal nitrogen is 3.7334 mg/L. The value is on the range. Therefore,
we can said that in that sample the amount of phosphorus is lower so the water does not polluted
and does not need any further treatment.

Table 2 is show the result of Ammoniacal Nitrogen from other groups (Result was taken
from Tun Teja’s group)

SAMPLE SAMPLE TITRATION NH3-N

VOLUME VALUE (mg/L)
(ml) (ML)
Blank (Distilled 1 65.00 0.90 0.0000
Water) 2 65.00 1.00 0.0000
3 65.00 1.10 0.0000
AVERAGE 65.00 1.00 0.0000
Water Sample 1 65.00 1.80 3.4462
(Section 7 Lake) 2 65.00 1.80 3.4462
3 65.00 2.00 4.3077
AVERAGE 65.00 1.87 3.7334
 The waste water samples was safely to be discharged. This is because surrounding of
section 7 lake does not have things that can cause higher concentration of ammoniacal nitrogen.
The water samples is very clean and safe to be used. Near to the water sample, there is no
factories that doing the Haber Process. Haber Process is for the manufacture of ammonia from
nitrogen and hydrogen. Waste water samples from section 7 are far from the factories. The
producing of ammonia at that area is lower than the standard.

The water samples also was compared with Water Quality Index (WQI). The water
sample has very high concentration of ammoniacal nitrogen. Water samples from section 7 was
categorized to the class IV in water quality index. Thus, the water samples require further
advance treatment in order to remove ammonia content of our water sample. Table 3 below
shown the Water Quality Index :

Table 3: Water Quality Index

Ammonia can be removed by a biological, fixed-film process that uses live bacteria to
oxidize the ammonia to nitrates and then simultaneously reduce the nitrates to nitrogen gas. Ion
exchange and adsorption material methods are simple to apply, cost-effective, environmentally
friendly technologies which are quite efficient at removing ammonium from treated water.
8. CONCLUSION
The ammoniacal nitrogen content in blank is 21.28 mg/L. While, the average
concentration in water samples from section 7 contains 1.12 mg/L. Based on the,
Environment Quality (Sewage) Regulation 2009 for new sewage treatment system the
water samples was not polluted. But, comparison with Water Quality Index, the water
samples was categorized to class IV and need further treatment.

9. REFERENCE

 Ammoniacal nitrogen. (2017, January 06). Retrieved April 16, 2019, from
https://en.wikipedia.org/wiki/Ammoniacal_nitrogen
 T., Loftus. (2003). Ammonia Nitrogen. Retrieved April 16, 2019, from
http://www.lagoonsonline.com/laboratory-articles/ammonia-nitrogen.htm
 Luo, X., Yan, Q., Wang, C., Luo, C., Zhou, N., & Jian, C. (2015, September 23).
Treatment of Ammonia Nitrogen Wastewater in Low Concentration by Two-
Stage Ozonization. Retrieved April 17, 2019, from
https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4586718/
 Nitrogen cycle. (2019, April 15). Retrieved April 27, 2019, from
https://en.wikipedia.org/wiki/Nitrogen_cycle
 Azreen, I., Lija, Y., & Zahrim, A. Y. (2017). Ammonia nitrogen removal from
aqueous solution by local agricultural wastes. IOP Conference Series: Materials
Science and Engineering,206, 012077. doi:10.1088/1757-899x/206/1/012077
 Emilie Spasov (2018). Ammonia-oxidizing archaea and complete ammonia-
oxidizing bacteria in a municipal wastewater treatment plant.
UWSpace.http://hdl.handle.net/10012/13925
APPENDIX

SOURCE : https://www.doe.gov.my/portalv1/wp-
content/uploads/2015/01/Environmental_Quality_Sewage_Regulations_2009_-_P.U.A_432-
2009.pdf