CMT 565

EXPERIMENT 6
LTM-PHOSPHORUS (P)

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
NAME OF LECTURER PUAN NORJANAH YURY
DATE OF EXPERIMENT 17 APRIL 2019
DATE OF SUBMISSION 8 MAY 2019
EXPERIMENT

LTM-PHOSPHORUS (P)

1. OBJECTIVE

a) To determine the concentration of phosphorus in the water sample taken.

b) To plot the graph of absorbance versus concentration of phosphorus
2. INTRODUCTION

Phosphorus (P) is a nutrient that is vital to human, animal, and plant growth. It is
one of the most common substances found in nature. It is a highly reactive, non-metallic
element existing in three allotropic forms, white, red and black. In its pure form, it is
toxic. Phosphorus occurs unnaturally in fertilizers that used in agriculture and
wastewater from household sewage. Phosphorus is found in water, solids and in the
bodies of biological organisms. Phosphorus in natural waters is usually found in the form
of phosphates (PO4-3) in the form of orthophosphate, inorganic form and organically
bound forms. Total Phosphorous is the sum of reactive, condensed and organic
phosphate.

Organic phosphate is phosphate that is bound to plant or animal tissue. Organic

phosphates are formed primarily by biological processes. They are contributed to sewage
and also may be formed from orthophosphates in biological treatment processes.
Inorganic phosphate is phosphate that is not associated with organic material. Types of
inorganic phosphate include orthophosphate and polyphosphates. Orthophosphate is
sometimes referred to as reactive phosphorus. Orthophosphate is produced by natural
processes and is found in sewage. Polyphosphates are strong complexing agents for some
metal ions. Polyphosphates are used for treating boiler waters and in detergents. In water,
polyphosphates are unstable and will eventually convert to orthophosphate.

High levels of phosphorus in nature can create algal blooms causing

eutrophication. Phosphorus was often found as the growth-limiting nutrient in fresh water
lakes and rivers. This is because the amount of phosphorus needed only least to the needs
of plants. Eutrophication is water have lots amount of minerals and nutrients which
induce excessive growth of algae. This process may result in oxygen depletion of the
water body. Eutrophication is often induced by the discharge of nitrate or phosphate-
containing detergents, fertilizers, or sewage into an aquatic system.
 The concentration of phosphates in aqueous solutions is typically expressed in
milligrams per liter of total P (or mg/L total P). Analytical techniques for determining
PO4-3 concentrations include volumetric, gravimetric, and colorimetric methods.
Spectrophotometry is a colorimetric method that is premised on the conformity of the
analyte solution to Beer’s laws. These laws, when combined, relate the concentration of a
chemical species in solution to the absorbance and transmittance of light energy that is
passed through the solution.

Phosphorus analyses embody two general procedural steps which is conversion of

the phosphorus form of interest to dissolved orthophosphate and colorimetric
determination of dissolved orthophosphate. Filter samples for determination of dissolved
reactive phosphorus, dissolved acid-hydrolyzable phosphorus and total dissolved
phosphorus through membrane filters. The analysis of different phosphorous forms of
particulate or organic-P is obtained by various pretreatment steps. Pretreatment may
consist of filtering to remove suspended matter or various digestion techniques designed
to oxidize organic matter.
3. LITERATURE REVIEW

There are many methods in determining the amount of phosphates in water such
as vanadomolybdophosphoric acid colorimetric method, stannous chloride method,
ascorbicmethod, automated ascorbic acid reduction method and some proposed method
such as flowinjection analysis for orthophosphate, manual digestion and flow injection
analysis for totalphosphorus and in-line UV/persulfate digestion and flow injection
analysis for totalphosphorus.The vanadomolybdophosphoric acid colorimetric method
works by forming heteropoly acid, molybdophosphoris acid through the reaction of
ammonium molybdateunder acid conditions. This procedure is done by adding a small
amount of vanadate-molybdate reagent into the sample water and using the colorimeter
under the wavelength of 400 - 470nm.

Phosphorus has been identified as a prime nutrient needed for algae growth in
inland environments. In 1992, the EPA reported that accelerated eutrophication was one
of the leading problems facing the Nation's lakes and reservoirs. Eutrophication caused
by the presence of excessive phosphorus (P) in the water bodies has received concerns
globally (Yang et al., 2008; Jarvie et al., 2006). Many algae blooms in rivers and lakes
are attributed to elevated phosphorus concentrations resulting from human activities.
Phosphorus as it commonly occurs in effluent. The main sources of P entering rivers are
sewage effluent and agricultural run-off (Bowes et al., 2015) with up to 70% being
attributed to sewage discharges (EA, 2015).

Phosphorus gets into water in both urban and agricultural settings. Phosphorus
tends to attach to soil particles and, thus, moves into surface-water bodies from runoff.
Phosphorus can also migrate with groundwater flows that was studied by USGS on Cape
Cod, Massachusetts. Since groundwater often discharges into surface water, such as
through streambanks into rivers, there is a concern about phosphorus concentrations in
groundwater affecting the water quality of surface water.
 Most of phosphorus compounds found in wastewater are water soluble. Biological
treatment uses biochemical processes to remove phosphorus. There is more phosphorus
in water than any biochemical technology can handle. Therefore, primary and secondary
waste water treatment can removes about 20-30% of phosphorus and phosphorus content
in pre-treated water is high above standard regulated limits. Not all local water
purification facilities have the phosphate removal ability and so new technologies need to
be designed to remove biogenic components from industrial and residential wastewaters.

Phosphorus removal techniques fall into three main categories which is physical,
chemical and biological. In a biological treatment plant, it is necessary to transfer
phosphate from liquid to the sludge phase, and the removal efficiency usually does not
exceed 30%, which means that the remaining phosphate should be removed by other
techniques. Chemical precipitation is also widely used for phosphate removal. The
precipitation of calcium phosphate from wastewater is an important physiochemical
process for phosphorus removal and it becomes increasingly significant for phosphorus
recovery since from the industry's viewpoint, it is far more promising to recover
phosphorus as calcium phosphates than other forms because it can be valorized in
agriculture as a slightly soluble fertilizer (Hosni, et al., 2007).

There are many methods in determining the amount of phosphates in water such
as vanadomolybdophosphoric acid colorimetric method, stannous chloride method,
ascorbicmethod, automated ascorbic acid reduction method and some proposed method
such as flowinjection analysis for orthophosphate, manual digestion and flow injection
analysis for total phosphorus and in-line UV/persulfate digestion and flow injection
analysis for tota lphosphorus.The vanadomolybdophosphoric acid colorimetric method
works by forming heteropoly acid, molybdophosphoris acid through the reaction of
ammonium molybdateunder acid conditions. This procedure is done by adding a small
amount of vanadate-molybdate reagent into the sample water and using the colorimeter
under the wavelength of 400 - 470nm.
4. MATERIALS AND APPARATUS

Apparatus Reagents
Colorimetric Equipment; UV/VIS Glass fibre filter paper
Spectrophotometer: PE 3110 Lambda 25
Acid-washed glassware Vanadate-molybdate reagent
Filtration apparatus Standard phosphate solution
Filter paper Phenolphthalein
Beaker 1N sodium hydroxide
Hot plate 1N sulphuric acid
Measuring cylinder Concentrated nitric acid
50ml of volumetric flask Concentrated sulphuric acid

5. METHODS

Filtration process:

a) Sample preparation

About 50ml of sample was measured into a volumetric flask. The sample then
was filtered using Whatman #40 filter paper into 50ml volumetric flask. Next, about
10ml of Vanadate-molybdate reagent (phosphorus reagent) was added into 50ml of
volumetric flask and was diluted to the mark with filtered sample. For blank, 10ml of
Vanadate-molybdate was added into 50ml of volumetric flask and was diluted to the
mark with distilled water. After 10 minutes, the absorbance of samples and a blank were
measured at a wavelength of 470nm using UV-Vis Lambda 25.

b) Preparation of calibration curve, 2mg/L to 15mg/L

About 5 of 50ml of volumetric flask were prepared. From the stock standard
phosphorus (50mg/L) about 2ml, 5ml, 10ml, 12ml and 15ml of stock standard
phosphorus was added into each of the volumetric flask. Then, about 10ml of phosphorus
reagent was added into each of the volumetric flask. Lastly, diluted all the standards up to
the mark with distilled water.

Digestion process:

a) Sample preparation

About 50ml of sample was added in a beaker. Then about 1ml of concentrated
sulphuric acid and 5ml of concentrated nitric acid were added into the beaker. Next, the
beaker was heated gently on a hot plate. The solution was evaporated to <10ml and was
allowed to cool. After that, 20ml of distilled water was added into the beaker. In addition,
1 drop of phenolphthalein was added. 1N of sodium hydroxide was added until colour
become pink tinge colour and 1N of sulphuric acid until it form colourless. About 10ml
of Vanadate-molybdate was added into the 50ml of volumetric flask and was diluted to
the mark with the sample. For blank, 10ml of Vanadate-molybdate was added into 50ml
of volumetric flask and was diluted to the mark with distilled water. After 10 minutes, the
absorbance of samples and a blank were measured at a wavelength of 470nm using UV-
Vis Lambda 25.

b) Preparation of calibration curve, 2mg/L to 15mg/L

About 5 of 50ml of volumetric flask were prepared. From the stock standard
phosphorus (50mg/L) about 2ml, 5ml, 10ml, 12ml and 15ml of stock standard
phosphorus was added into each of the volumetric flask. Then, about 10ml of phosphorus
reagent was added into each of the volumetric flask. Lastly, diluted all the standards up to
the mark with distilled water.
6. RESULTS

Tasik Shah Alam Seksyen 7

Concentration (mg/L) Absorbance

Blank 0.000
2 0.028
5 0.078
10 0.171
12 0.205
15 0.255
Sample (filtration) 0.054
Sample (digestion) 0.062

Graph absorbance vs concentration phosphorus of water samples section 7

Graph Absorbance versus Concentration

0.3

0.25 y = 0.0173x - 0.0042

R² = 0.9991
0.2
Absorbance,A

0.15

0.1

0.05

0
0 2 4 6 8 10 12 14 16
-0.05
Concentration (mg/L)

From graph, concentration of sample (filtration) = 3.62 mg/L

From graph, concentration of sample (digestion) = 4.20 mg/L
7. DISCUSSION

The removal of phosphorus (P) from domestic wastewater is primarily to reduce

the potential for eutrophication in receiving waters and is mandated and common in many
countries. Controlling phosphoros discharged from municipal and industrial wastewater
treatment plants is a key factor in preventing eutrophication of surface waters.
Phosphorous is one of the major nutrients contributing in the increased eutrophication of
lakes and natural waters. The water samples is compared with Environment Quality
(Sewage) Regulation 2009. Two standards for effluent discharge which is Standard A and
Standard B. Water sample from section 7 was compared with Standard B based on table
1. This is because Standard B for discharge downstream of any raw water intake. The
Standard B shows that the value for phosphorus was 10 mg/L.

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

Phosphorus is very useful and effective as a fertiliser to encourage plant growth, it

can cause catastrophic problems if too much gets into our streams, rivers, lakes and seas.
Phosphorus reaches bodies of water via runoff over land, leaching through soil from
fertilisers and discharges from sewage treatment works. In fact, the UK Water Industry
Research (UKWIR) cites phosphorus as a major reason that UK rivers are not achieving
good status under the Water Framework Directive (WFD).

In this experiment, the phosphorus of water sample section 7 was calculated. The
phoshorus reading for water samples was obtained from the absorbance versus
concentration graph. The phoshorus reading for water samples section 7 for sample
(filtration) and sample (digestion) is 3.63 ppm and 4.20 ppm. This phosphorus content
reading in the sample is lower compared to Standard B for effluent discharge. The
Standard B shows that the value for phosphorus was 10 mg/L. The result is lower than
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 Phosphorus from other group (Result was taken from
NurFarrah Atiqah’s group)

Sample Tasik Shah Alam Section 7 Concentration of phosphorus (ppm)

Sample (filtration) 3.57 ppm
Sample (digestion) 4.45 ppm

Based on result from other groups, the The phoshorus reading for water samples
section 7 for sample (filtration) and sample (digestion) is 3.57 ppm and 4.45 ppm.
Therefore, the result was still lowered compared to the Standard B. Therefore, it prove
that the water sample from section 7 was not polluted with phosphorus.

Water sample from section 7 was not polluted with phosphorus because the water
is for recreational. Phosphorus is an essential element for plant life, but when there is too
much of it in water, it can speed up eutrophication of rivers and lakes. Moreover, around
the lake there is no farm that can induced phosphorus in the form of phosphate.Plant only
need least amount of phosphorus only. The causes of higher level of phosphorus in water
is the use of fertilisers. Next, the factory is far away from the lake and there is no
agricultures activity around it.
 The effectiveness of phosphorus removal during wastewater treatment can
depending on and the treatment methods used. There are two methods of removing
phosphorus from wastewater which is biological removal and chemical removal.
Biological phosphorus removal can be achieved by cycling the activated sludge in
anaerobic and aerobic conditions which can build up a population of microorganisms that
are capable of storing phosphorus intracellularly as polyphosphate. A much simpler
method of removing phosphorus can be carried out by dosing a metal-based coagulant
into the wastewater.
8. CONCLUSION

As for the conclusion, both concentration of sample (filtration and digestion) in lake
section 7 is 3.62 ppm and 4.20 ppm was taken from the absorbance versus concentration
graph.

9. REFERENCE
 S., Murphy. (2007, April 27). General Information on Phosphorus. Retrieved May
5, 2019, from http://bcn.boulder.co.us/basin/data/COBWQ/info/TP.html
 Ortho Phosphorus in Water. (n.d.). Retrieved May 5, 2019, from
https://www.asaanalytics.com/ortho-phosphorous.html
 Novin. (2019, April 29). Phosphorus. Retrieved May 5, 2019, from
https://mitreh.com/en/phosphorus/
 Bunce, T., J., Ndam, Edmond, Irina, Moore. (2018, January 26). A Review of
Phosphorus Removal Technologies and Their Applicability to Small-Scale
Domestic Wastewater Treatment Systems. Retrieved May 5, 2019, from
https://www.frontiersin.org/articles/10.3389/fenvs.2018.00008/full#B32
 Rparajas13. (n.d.). Phosphate.2.docx - 1 Chapter 1 INTRODUCTION Phosphorus
is the eleventh most abundant element in earth and is one of the twenty most
abundant element in. Retrieved May 5, 2019, from
https://www.coursehero.com/file/31598462/phosphate2docx/
APPENDIX

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