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Module code:CIVE2012Y(3)
REMARKS
UNIVERSITY OF MAURITIUS
COURSEWORK:
LAB REPORTS ON WASTEWATER PRACTICALS
By:
HOW YUEN SIONG Yannick Van Pow-1310446
AJODAH Trisha Ooshita Devi-1310754
KISTO Chusnee- 1312452
BUNDHOO Akshay- 1314463
LUBRUN Veeresh Kumar- 1314488
Table of Contents
List of Tables ................................................................................................................................................ 7
List of Figures ............................................................................................................................................... 8
1.0 Introduction ............................................................................................................................................. 9
2.0 Biological Oxygen Demand .................................................................................................................. 10
Abstract ....................................................................................................................................................... 10
2.0.1 Introduction ........................................................................................................................................ 10
2.0.1.1 Aims-........................................................................................................................................... 10
2.0.2 Literature Review............................................................................................................................... 10
2.0.3 Methodology ...................................................................................................................................... 11
2.0.4 Data Collection & Analysis ............................................................................................................... 14
2.0.5 Discussion .......................................................................................................................................... 14
2.0.6 Conclusion ......................................................................................................................................... 15
References ................................................................................................................................................... 15
3.0 Chemical Oxygen Demand ................................................................................................................... 16
Abstract ....................................................................................................................................................... 16
3.0.1 Introduction ........................................................................................................................................ 17
3.0.1.1 Aim and objectives ..................................................................................................................... 17
3.0.2 Literature Review............................................................................................................................... 18
3.0.3 Methodology ...................................................................................................................................... 19
3.0.4 Data Collection .................................................................................................................................. 21
3.0.5 Data Analysis ..................................................................................................................................... 22
3.0.6 Conclusion ......................................................................................................................................... 23
References ................................................................................................................................................... 23
4.0 Solids .................................................................................................................................................... 24
3
5.1.1.1Aims ............................................................................................................................................. 34
5.1.2 Literature Review............................................................................................................................... 34
5.1.3 Methodology ...................................................................................................................................... 35
5.1.3.1 Principle ...................................................................................................................................... 35
5.1.3.2 Health and Safety ........................................................................................................................ 37
5.1.4 Data Collection .................................................................................................................................. 37
5.1.5 Data Analysis ..................................................................................................................................... 37
5.1.6 Discussion .......................................................................................................................................... 38
5.1.6.1 Limitation.................................................................................................................................... 38
5.1.7 Conclusion ......................................................................................................................................... 38
References ................................................................................................................................................... 38
5.2 Nitrate ................................................................................................................................................... 39
Abstract ....................................................................................................................................................... 39
5.2.1 Introduction ........................................................................................................................................ 39
5.2.1.1 Aims ............................................................................................................................................ 39
5.2.2 Literature Review............................................................................................................................... 39
5.2.3 Methodology ...................................................................................................................................... 40
Apparatus ............................................................................................................................................ 40
5.2.3.1 Health and Safety Issues ............................................................................................................. 40
5.2.4 Data Collection and Analysis ............................................................................................................. 41
5.2.5 Conclusion ......................................................................................................................................... 41
5.3
Phosphorus ...................................................................................................................................... 42
Abstract ....................................................................................................................................................... 42
5.3.1 Introduction ........................................................................................................................................ 42
5.3.1.1 Aim ............................................................................................................................................. 42
5.3.2 Literature Review............................................................................................................................... 43
5.3.3 Methodology ...................................................................................................................................... 43
5
Sulfate ............................................................................................................................................. 46
Abstract ....................................................................................................................................................... 46
5.4.1 Introduction ........................................................................................................................................ 46
5.4.1.1 Aims ............................................................................................................................................ 46
5.4.2 Literature Review............................................................................................................................... 46
5.4.3 Methodology ...................................................................................................................................... 47
5.4.3.1 Principle ...................................................................................................................................... 47
5.4.3.2 Health and Safety ........................................................................................................................ 48
5.4.4 Data Collection and Analysis ............................................................................................................. 48
5.4.5 Discussion .......................................................................................................................................... 48
5.4.5.1 Limitations .................................................................................................................................. 48
5.4.6 Conclusion ......................................................................................................................................... 49
REFERENCES ........................................................................................................................................... 49
5.5 Chloride................................................................................................................................................. 50
5.5.1 Introduction ........................................................................................................................................ 50
5.5.1.1 Aims and Objectives ................................................................................................................... 50
5.5.2 Literature Review............................................................................................................................... 50
5.5.3 Methodology ...................................................................................................................................... 51
5.5.3.1 Health and Safety ........................................................................................................................ 51
5.5.4 Data Collection .................................................................................................................................. 51
5.5.5 Data Analysis ..................................................................................................................................... 52
5.5.6 Discussion .......................................................................................................................................... 52
5.5.7 Conclusion ......................................................................................................................................... 52
6
References ................................................................................................................................................... 52
6.0 pH.......................................................................................................................................................... 53
Abstract ....................................................................................................................................................... 53
6.0.1 Introduction ........................................................................................................................................ 53
6.0.1.1 Aims ............................................................................................................................................ 53
6.0.2 Literature Review............................................................................................................................... 53
6.0.3 Methodology ...................................................................................................................................... 54
6.0.4 Data Collection .................................................................................................................................. 54
6.0.5 Conclusion ......................................................................................................................................... 54
7.0
List of Tables
Table 2.1-BOD for blanks........................................................................................................................... 14
Table 2.2- BOD for wastewater sample ...................................................................................................... 14
Table 3.1: Volume of FAS for the titration against digested sample. ......................................................... 21
Table 3.2: Volume of FAS for the titration against digested blank. ........................................................... 21
Table 3.3: Volume of FAS for the titration against undigested blank. ....................................................... 21
Table 3.4 : Mean volume of FAS used for digested sample. ...................................................................... 22
Table 3.5 : Mean volume of FAS used for digested blank.......................................................................... 22
Table 3.6: Mean volume of FAS used for undigested blank...................................................................... 22
Table 4.1: Types of Solids (Adapted from Wastewater lab sheet, 2015).................................................... 24
Table 4.2 : Results of weights for suspended solid ..................................................................................... 27
Table 4.3: Determining total suspended solids ........................................................................................... 27
Table 5.1: Concentration of Nitrate in sample. ........................................................................................... 41
List of Figures
Figure 2.1: Recommended sample volumes for the 5-day biochemical oxygen demand test .................... 12
Figure 4.1: Imhoff cone .............................................................................................................................. 31
Figure 4.2: Reading of volume of solid that has settled .............................................................................. 31
Figure 5.1: Spectrophotometer .................................................................................................................... 36
Figure 5.2: The Filtration Apparatus........................................................................................................... 44
Figure 5.3: Blue colour showing presence of phosphorus .......................................................................... 44
Figure 5.4: Spectrophotometer .................................................................................................................... 47
Figure 8.1: Digit multiplier for sample volume and Titration Cartridge (N Hg (NO3)2) ........................... 56
Figure 8.2: Typical Composition of Untreated Domestic wastewater ........................................................ 57
1.0 Introduction
Wastewater treatment methods are characterized by main categories which are physical, chemical and
microbiological. The aim of the experiments carried out were to assess the quality of a given wastewater
sample with respect to the aforementioned categories. The experiments conducted mostly investigated the
wastewater quality for the safe disposal on land and in receiving water bodies. The physical
characteristics included the constituents of wastewater as related to amount and type of solids present.
Among the chemical characteristics included the investigation of the chemical oxygen demand, dissolved
salts and pH of the wastewater.
The wastewater effluent characteristic is defined against a standard, promulgated by the legislation in a
particular country. In Mauritius, threshold values are derived locally from The Environment Protection
Act, 2002 to ensure the safety of the general public health.
In Mauritius, the enforcing agencies of these standards are the Ministry of Health, Water Resources Unit
and the Waste Water Agency. Laboratory tests are conducted by the Central Water Authority to ensure
that wastewater for disposal and reuse meet the required standards.
Abstract
This experiment was conducted on a wastewater sample where its Biochemical oxygen demand (BOD)
was obtained after a period of 7-days. Dissolved oxygen (DO), in three BOD bottles filled with the
sample and was diluted with two different dilution factors, were measured. The measurement of DO in
blanks containing only dilution water was also carried out. The values of DO in the blanks and diluted
samples fluctuated slightly and could be therefore be accepted. The bottles used in the experiment were
not all of 300 ml and this would have induced errors in the values.
2.0.1 Introduction
The concentration of organic matter in waste water samples is often expressed in terms of
Biological oxygen demand (BOD). The BOD5 test procedure is based on the amount of dissolved oxygen
used by microorganisms in the water. As the amount of organic matter in sewage increases, the more
oxygen will be utilised by microorganisms to degrade dumping sewage which would therefore indicate
high BOD value. Digestion of these organic compounds in neutral ecosystem such as lakes, rivers can
deplete available oxygen and result in fish asphyxiation.
2.0.1.1 AimsTo determine the BOD of the wastewater sample
10
the amount of DO available in the air-saturated BOD5 sample (American Public Health Association and
others, 1995).
The following criteria have to be met for the BOD5 values to be accepted:
The DO concentration after 5 days must be at least 1 mg/L and at least 2 mg/L lower in
concentration than the initial DO (American Public Health Association and others, 1995).
At least three different dilutions are set per sample to cover the anticipated range of BOD. The
three sample volumes used are selected to provide an overlapping range in expected BOD
concentrations. Because bacteria need nutrients and micronutrients to survive, these compounds
are added to the dilution water.
Similarly, the pH of the dilution water needs to be maintained in a range suitable for bacterial
growth (6.5 to 7.5). Some types of sewage, such as untreated industrial wastes, disinfected
wastes, and wastes that have been heated to a high temperature contain too few bacteria to
perform the test. Thus, the samples must be seeded with a population of microorganisms to
produce an oxygen demand. Most natural waters contain an adequate amount of microorganisms.
For guidance on seeding procedures, including the BOD5 equation when dilution water is seeded,
refer to American Public Health Association and others (1995).
2.0.3 Methodology
Apparatus
Pipettes
Measuring cylinders
BOD Incubator
Standard flask
Magnetic stirrer
Stir bar
Glass funnel
11
Gloves
Tissue paper
Reagents
Nutrient Solutions:
Procedure
The following preparations are needed before implementing the BOD test procedure:
1. The dilution water was prepared before initiating BOD tests.
2. A glass jar was filled with 900 ml of dilution water and was aerated dilution water before addition
of nutrient solutions. After aeration, 1 mL each of the potassium phosphate, magnesium sulfate,
calcium chloride, and ferric chloride solutions per 1 L of dilution water was added to dilution
water.
Figure 2.1: Recommended sample volumes for the 5-day biochemical oxygen demand test
The COD obtained was 179 mg/L. It was assumed that the value for BOD will be half that of
COD, i.e.89 mg/L.
From Table 1, the two BOD5 ranges for our sample were within two ranges: 30-105 and 60210. Therefore two sets of samples with different dilution factors will be tested.
300
300
20
= 15
300
10
= 30
For the test, 3 samples were to be prepared for each set of dilution factor. A measuring
cylinder was filled with 900 ml of dilution water in order to fill 3 bottles, the sample size was
determined with D.F. equals to 15:
Sample size: 900/D.F.= 900/15= 60 ml
With dilution factor equals to 30, Sample size = 900/30 = 30 ml
4. The sample was poured from the pipet into clean BOD bottles. Dilution water filled the remaining
portion of the BOD bottle. Three other samples were prepared with the other dilution factor.
5. Three samples containing only dilution water were prepared in order to serve as blanks for quality
control. Two of the three samples had to meet the blank-water criterion in order for the data to be
accepted.
6. Each bottle was labelled. The initial DO concentration (D1) of each sample and each dilution
blank was measured. To avoid entrapment of air, the self-stirring sensor was carefully inserted
into the BOD bottle. The stirrer was turned on and allowed 1 to 2 minutes for the DO reading to
stabilise.
7. The stirrer was turned off and the sensor removed from the BOD bottle.
8. The sealed BOD sample was placed in the air incubator at 20C 1C. With the advice of the lab
technician, instead of measuring the BOD after five days, we would determine the BOD after
seven days because the BOD at five days would be quite small.
9. At the end of 7 days, the BOD bottles were removed from the incubator, the over-caps were took
off, removing the ground-glass stopper, and measuring the final DO concentration (D2).
13
Initial DO
reading (D1)
Final DO reading
(D2)
BOD (D1-D2)
B1
8.1
7.4
0.7
B2
8.1
6.9
1.2
B3
8.1
7.0
1.1
BOD average
(mg/L)
1.0
Bottle
S1-1
S1-2
S1-3
S2-1
S2-2
S2-3
Dilution
Factor
15
30
Environmental sample
Initial DO
Final DO
reading (D1)
reading (D2)
7.1
4.4
7.1
5.6
6.9
5.3
7.9
5.5
8.3
5.2
7.7
5.3
BOD
[(D1-D2)/P]
14
7.5
8.0
24
31
24
BOD average
(mg/L)
9.8
26
2.0.5 Discussion
Some irregularities in the BOD may be caused due to the fact that some of the BOD bottles used were of
250 ml size and not 300 ml as it should.
14
2.0.6 Conclusion
The BOD of the wastewater sample would be well within limits imposed by regulations in the EPA 2002
act.
References
1. Amrita.vlab.co.in, (2015). Biological Oxygen Demand (Theory) : Ecology Virtual Lab :
Biotechnology and Biomedical Engineering : Amrita Vishwa Vidyapeetham Virtual Lab. [online]
Available at: http://amrita.vlab.co.in/?sub=3&brch=272&sim=1430&cnt=1 [Accessed 1 Apr.
2015].
2. S.W, M. and G.C., D. (n.d.). FIVE-DAY BIOCHEMICAL OXYGEN DEMAND. 3rd ed. [ebook]
Available
at:
https://water.usgs.gov/owq/FieldManual/Chapter7/NFMChap7_2_BOD.pdf
15
Abstract
In this experiment the first step was to allow the sample to stand for some time for decantation. The
specified volume of reagent and decanted sample was transferred to digested tube. The same procedure
was done but instead of decanted sample, distilled water was used. The digested sample and digested
blank was prepared and placed into a fume hood. After waiting for 2 hours the tubes was removed from
the fume hood and allowed to cool down. In the meantime, the undigested blank was prepared directly in
a conical flask. The digested tubes were each transferred to a labelled conical flask with the addition of
distilled water that was used for washing the tube. The mixture in the conical flasks was then titrated
against Ferrous Ammonium Sulphate after addition of indicator. The end point of the titration was
reached when colour of mixture became reddish brown. The COD was then calculated in mg/L.
16
3.0.1 Introduction
The COD test measures the oxygen demand for the decomposition of organic compounds and oxidation
of inorganic chemicals (ammonia and nitrite) using strong chemical oxidation while the Biological
oxygen demand test is the amount of dissolved oxygen required by microorganism to break down organic
matter. Thus COD value is higher than BOD value.
The advantages of the COD test as compared to the BOD test are:
The major disadvantage of the COD test is that the results are not directly applicable to the 5-day BOD
results.
The COD gives an indication of how polluted the water is and the water quality. The COD test is usually
carried out for both influent and effluent. Hence, the efficiency of a treatment can be determined by
expressing it in term of the percentage removal of COD.
3.0.1.1 Aim and objectives
Aim: To determine the Chemical Oxygen demand in mg/L.
Objectives:
To do titration of digested solutions and undigested blank against FAS so that titre value is within
0.2ml.
17
Where
B= Mean volume of FAS used for digested blank (ml)
S= Mean volume of FAS used for digested sample (ml)
T= Mean volume of FAS used for undigested blank (ml)
D= Dilution factor of sample.
18
3.0.3 Methodology
Apparatus:
Autopipette
Reagents
Digestion reagent
Catalyst solution
Ferroin indicator
Procedure
Preparation of sample
1. Approximately 800 ml of the sample was poured into a beaker.
2. The beaker was allowed to stand for 30 minutes.
3. The sample in the beaker was decanted into another clean beaker. The decanted sample was used
for the COD test.
Preparation of digested sample:
1. 1.5 ml of the digested was dispensed into the digested tube.
2. 2.5 ml of the decanted sample was measured using an autopipette and transferred to the tube.
3. 3.5 ml of the catalyst was added to the tube. Prior to addition of catalyst, care was taken to hold
the upper part of the tube as the mixture becomes hot on addition of catalyst.
4. The cap was then placed onto the tube and then closed tightly.
5. The mixture was mixed by slightly tilting the digested tube. Solution in the tube was yellow.
6. The digested tube was then labelled and placed in the tube rack
7. The procedure 1 to 6 was repeated for 2 addition tube.
19
Both the digested blank tubes and the digested sample tubes were placed in a fume hood for 2
hours.
After 2 hours, the 6 tubes were removed from the fume hood using heat resistant gloves.
While the tubes were allowed to cool, the undigested blanks were prepared.
20
Titration procedure:
1. The burette was filled with Ferrous Ammonium Sulphate (FAS) using a funnel. The initial burette
reading was noted.
2. 2 drops Ferroin indicator was added to the undigested blank. On addition was colour of mixture
changed to yellow.
3. The mixture was then titrated against Ferrous Ammonium Sulphate (FAS) until the colour change
in conical flask from yellow to bluish green to finally reddish brown.
4. The final burette reading was then noted.
5. The step 1 to 4 was repeated for the 9 remaining conical flask.
Titration Number
11.50
22.80
34.00
0.00
11.70
22.80
11.50
11.10
11.20
Table 3.2: Volume of FAS for the titration against digested blank.
Titration Number
13.60
27.45
41.20
0.00
13.60
27.50
13.60
13.85
13.70
Table 3.3: Volume of FAS for the titration against undigested blank.
Titration Number
14.35
28.30
42.20
0.30
14.35
28.30
14.05
13.95
13.90
21
Titration Number
Volume of FAS used/ cm
11.50
11.10
11.20
11.15
Titration Number
Volume of FAS used/ cm
13.60
13.85
13.70
13.65
Titration Number
Volume of FAS used/ cm
14.05
13.95
13.90
Where
B= Mean volume of FAS used for digested blank (ml)
S= Mean volume of FAS used for digested sample (ml)
T= Mean volume of FAS used for undigested blank (ml)
D= Dilution factor of sample.
D= 1 as sample was not diluted
COD=
..
13.97
= 178.95
= 179 mg/L
22
3.0.6 Conclusion
According to the Environmental Act 2002, the maximum permissible limit for discharge of sewages in
surface water, lands and ocean is 120 mg/l. The COD value is 179 mg/l. So this sample requires treatment
prior to discharge.
The COD value obtained is very important to estimate the Biological Oxygen demand. The BOD is
estimated to be about 50 percent of the COD so that a dilution factor for the BOD test can be obtained.
With the ratio of COD to BOD, the waste water can be classified as industrial or municipal. The ratio will
also dictate the treatment required.
References
1. Chemical Oxygen Demand (COD) Testing Procedures. Available at:
http://water.me.vccs.edu/courses/ENV149/cod.htm Access on 28 March 2015
2. Difference Between BOD and COD. Available at:
http://www.differencebetween.com/difference-between-bod-and-vs-cod/ Access on 30 March
2015
3. Hanna instrument, Chemical Oxygen demand. Available at:
http://www.hannainst.com/usa/subcat.cfm?id=008 Access on 28 March 2015
4. Wayne Bolyes, The Science of chemical oxygen demand [pdf], Booklet No. 9. Available at:
file:///C:/Users/user/Downloads/Science%20of%20Chemical%20Oxygen%20Demand.pdf
Access on 28 March 2015
23
4.0 Solids
All contaminants of water, other than dissolved gases, contribute to the solids concentration therefore it is
an important in indicator of the overall quality and potential polluting power of the water. Solids content
is also a useful parameter for the design and operation of wastewater treatment. The type of solid
concentration can be confusing due to the various different terms used, some are summarised below.
Table 4.1: Types of Solids (Adapted from Wastewater lab sheet, 2015)
Solid type
Suspended solid
Description
Particulate solid in
suspension
(of varying size)
Solids in solution and fine
colloidal particles will pass
through a GF/C filter paper
TS=SSDS
24
Method
Filter sample through GF/C
filter paper and dry at 105c
Filter out SS as above and
place filtrate in a crucible and
evaporate to dryness
Place sample in crucible and
evaporate to dryness
Heat dried solids at 550 for
2 hours
Place 1L of sample in an
Imhoff cone and allow to
settle for 30 minutes
4.1.3 Methodology
Apparatus used:
Measuring cylinders
Whatman GF/C Filter papers
Drying oven, 103- 105 C
Dessicators
Analytical balance, accuracy 0.0001mg
Filtration apparatus
Vacuum pump
Procedure:
1. Three filter papers were placed into the holder and suction was applied. After the filter papers
were washed with 3 successive volumes of distilled water, they were dried in an oven for 1 hour
and then stored in a dessicator.
2. Each filter paper was carefully and accurately weighed on an electronic balance reading to 4
decimal place using a pair of tweezers. The filter paper was then placed onto the filter holder.
3. After mixing the water sample, 250 ml of the sample was measured from measuring cylinder and
about 20 ml of sample was added to the filter paper in succession until filtration slowed while
suction was applied.
4. When all the 250ml of sample had been filtered, air was allowed to pass through the collected
solids for a further 30s and then suction was stopped.
5. The filter paper was removed and placed in petri dish together with residue. The filter paper was
then placed in an oven for 1 hour.
6. Procedure 3 to 5 was repeated for the other two filter papers.
7. After 1 hour the three filter papers were removed and dried in a dessicator.
8. Each filter was then weighed and allowed to cool further in the dessicator. At 5 minutes interval
the filter papers were re weighed until a constant weight was recoreded.
4.1.3.1 Precautions
The filter paper should be allowed to dry for some time before placing it in the petri dish to avoid
sticking of the filter paper to the bottom of the petri dish after drying in oven.
Use a pair tweezers to handle the filter paper at any time during the experiment.
26
Slip resistant shoes should be worn at all time during the course of the experiment.
The vacuum pump device should not be handle with wet hands due to risk of electric shocks.
Heat proof gloves should be used to remove the filter papers from the oven.
Beakers, filter holder and petri dishes should not be manipulated with wet hands as they are
fragile glass wears and can cause injury if broken.
The temperature should be verified that it is set at 105 to avoid ignition of the filter paper.
Filter
paper
Weight of filter
paper after drying/g
1
2
3
0.3514
0.3502
0.3468
Filter
paper
1
2
3
Weight of
filter paper
after drying/g
(A)
0.3514
0.3502
0.3468
Mass of filter
after 1 hour/g
W1
0.3745
0.3640
0.3725
After 5
minutes
interval/g
W2
0.3744
0.3639
0.3725
27
Final
mass/g
(B)
Mass of
suspended
solids/g (B - A)
Suspended
solids/(mg/L)
0.3745
0.3640
0.3725
0.0231
0.0138
0.0257
Average/(mg/L)
92.4
55.2
102.8
125.2
Suspended solids =
B A 1000
C
4.1.6 Discussion
The filter papers are heated for one hour to ensure that all water have been removed and then is allowed to
cool until a constant mass is obtained. The Environment Protection Act, 2002 sets a permissible limit of
300 mg/l and 35 mg/l for effluent discharge into the ocean and surface water respectively. The wastewater
sample cannot be disposed into surface water since it exceeds the maximum permissible amount. From
table 11.2, the value of 125.2mg/l suggests that the wastewater sample might have been taken from an
untreated domestic wastewater with a low concentration of suspended solid.
3.1.7 Limitations
It was difficult to obtain a homogenous solution of suspended solids as they either settle down
quickly after mixing or they get decanted while pouring in the measuring cylinder.
The time taken for filtration to take place was not considered since longer time taken for filtration
to place indicates clogging of the filter paper.
4.1.7 Conclusion
The amount of suspended solid in the sample exceeds the allowable amount of suspended solid for
discharge in surface water. Therefore, the wastewater has to undergo further treatment if it is to be
discharged in surface water to avoid any reduction in dissolved oxygen. However, the sample meets the
required standard, in terms of suspended solids, to be disposed in the ocean as set by the Environmental
Protection Act.
28
References
1. Barbara H., 1996, Practical Manual of Wastewater Chemistry, Lewis Publishers, CRC press,
United States of America.
2. Mackenzie, L.D, 2010, Water and Wastewater Engineering: Design, Principle and Practice, The
McGraw-Hill, Inc., United States.
29
Abstract
Settleable solids are that portion of the suspended solids which are of sufficient size and weight to settle
in a given period of time, usually one hour. The test was carried out in an Imhoff cone and the volume of
solids obtained was 2.75 ml/l.
4.2.1 Introduction
The term Settleable Solids refer to solids in suspension that will settle, under quiescent conditions, under
the influence of gravity. For example, in wastewater, sludges are accumulations of Settleable Solids. The
measurement of Settleable Solids is important in practice to determine the efficiency of sedimentation
units and to deduce the physical behaviour of waste streams entering natural bodies of water.
4.2.1 Aim
The main aim of this practical is to measure the amount of Settleable Solids in the sample.
30
4.2.3 Methodology
Apparatus used
a) Imhoff cone
b) 1 L measuring cylinder
c) Long glass rod
Procedure
1. The sample of wastewater was mixed very well and 1 litre of the sample was measured using a
measuring cylinder.
2. The 1 litre sample was rapidly poured into the Imhoff cone and the solids were allowed to settle
for 30 minutes.
3. After 30 minutes, a glass rod was used to ease off the solids which had stick to the wall of the
Imhoff cone using a long glass rod.
31
4. After further 30 minutes, the volume of solids that have settled is read off from the Imhoff cone
and recorded.
4.2.3.1 Precaution
Care was taken to avoid moving the Imhoff cone while using the glass rod so as not to disturb the settling
process.
References
1. SAWYER, C.N., MCCARTY, P.L. AND PARKIN, G.F., 2003. Chemistry for environmental
engineering and science. 5th ed. New York: McGraw Hill.
32
33
5.1 Ammonia
Abstract
In this experiment, the concentration of ammonia in the water sample was determined by the Nesslers
method. Polyvinyl Alcohol Dispersing agent, Nessler Reagent as well as mineral stabilizer were added in
the water sample. This resulted in a yellow colour of the solution which was then related to the ammonia
concentration.
5.1.1 Introduction
Ammonia is produced as a result of microbiological actions on nitrogenous organic matter. A higher
concentration of ammonia is found in waters polluted by industrial discharge, ammonium salts and
fertilizers. Ammonia is also produced by the anaerobic reduction of the nitrogen compounds in water.
There are two forms of ammonia nitrogen in water which are free ammonia and ammonium ions. Their
respective proportions in water depend on the pH.
5.1.1.1Aims
To determine the concentration of ammonia by the Nesslers method.
34
Nitrite: 1 mg/L
Nitrate: 10 mg/L
Ammonia can be separated from water by several treatment techniques. These include:
Ion exchange
Membrane separation
Adsorption and
Air stripping
5.1.3 Methodology
5.1.3.1 Principle
In this method, the mineral stabilizer is added to form complexes with hardness causing agents. The
Polyvinyl Alcohol Dispersing Agent is added to aid in the formation of the yellow colour resulting from
the reaction between Nessler Reagent and ammonium salts. The yellow colour formed is proportional to
ammonia concentration.
Apparatus and Reagents
The equipment and reagents used are:
(a) DR 2000 Spectrophotometer
(b) Measuring cylinders
(c) Sample matching cells
(d) Nessler Reagent
(e) Mineral stabilizer
(f) Polyvinyl Alcohol Dispersing Agent
35
Procedure
1. The stored program number for ammonia nitrogen (NH3- N) was entered.
The number 3 8 0 was entered and the READ/ENTER button was pressed.
The display showed: DIAL nm TO 425.
2. The wavelength dial was rotated until the small display showed 425nm.
3. The READ/ENTER button was pressed.
The display showed: mg/l N NH3- Ness.
4. A 25 ml graduated mixing cylinder was filled to the 25 ml mark with the sample.
5. Another 25 ml mixing graduated cylinder was filled with deionized water (the blank).
6. Three drops of Mineral Stabilizer was added to each cylinder.
7. Each cylinder was inverted several times to mix the sample properly.
8. Three drops of Polyvinyl Alcohol Dispersing Agent was added to each cylinder.
9. Each cylinder was again inverted several times to mix the sample properly.
10. 1.0 ml of Nessler Reagent was pipetted into each cylinder.
11. A stopper was placed on the top of each cylinder and they were then inverted to mix the sample.
12. The SHIFT TIMER was pressed and a 1-minute reaction period began.
13. Each solution was poured into a sample cell.
14. When the timer beeped, the display showed mg/l N NH3- Ness.
15. The blank was placed into the cell holder and the light shield was closed.
16. Furthermore, the zero button was pressed.
The display showed: WAIT and then 0.0 mg/l N NH3- Ness.
36
17. The prepared sample was placed into the cell holder and the light shield was closed.
18. The READ/ENTER button was pressed.
The display showed: WAIT and then the result in mg/l ammonia expressed as ammonia nitrogen
(NH3- N) was displayed.
5.1.3.2 Health and Safety
Wear hand gloves to avoid any contact between the skin and the chemicals used in order to avoid
burns.
Wear adequate shoes to protect the feet and also to avoid slipping in case the floor is wet.
37
5.1.6 Discussion
The concentration of ammonia in the wastewater sample is found to be 35.4 mg/L NH3- N. Since this
concentration is higher than the permissible limit of 1.0 mg/L as stated in the Environment Protection
Act, the wastewater sample cannot be discharged directly into the environment. It should be treated
accordingly to reduce the concentration of ammonia. It represents a risk to the flora and fauna and is
likely to cause eutrophication problems.
5.1.6.1 Limitation
Fingerprints on the sample cell affected the reading obtained from the spectrophotometer since it affected
the light intensity passing through the sample. Hence the fingerprints are considered to be a source of
error in the experiment.
5.1.7 Conclusion
It can be concluded that it is necessary to treat the sample of wastewater to reduce the ammonia
concentration prior to discharging it since the ammonia concentration in the sample is higher than the
maximum permissible limit.
References
1. Howard S Peavy, Donald r, Rowe George tchobanoglous, 1985, Environmental engineering, Mc
Graw Hill book company, USA
2. The importance of maintaining wastewater quality. [ONLINE]. Available at:
http://www.wateronline.com/doc/the-importance-of-maintaining-wastewater-qual-0001 Accessed
on 28th March 2015.
38
5.2 Nitrate
Abstract
In this test, the sample provided was first filtrated after the addition of activated carbon in the sample. The
stored number for nitrate was entered for the spectrophotometer and dialled to 500nm. The sample cell
was then filled with 25ml of filtered sample and one Nitra Ver 5 Nitrate Reagent Powder pillow. The
mixture was shaken for 1 minute and left to stand for further 5 minutes. In the meantime, the blank was
prepared which consist of only the filtered sample. The blank was first placed in the spectrophotometer to
calibrate it to zero. The sample cell containing the sample and reagent was then placed in the cell holder
to get the concentration of Nitrate in mg/l.
5.2.1 Introduction
Nitrate are essential element for plants however, in excess concentration, the quality of water is affected.
High level of nitrate in water may lead to eutrophication which in term cause the accelerated growth of
algae and result in water that cannot sustain life. The main source of nitrates in water is fertilisers.
Waste water usually contains high concentration of nitrates. So the water cannot be directly disposed in
surface water or land. This test is essential to find the nitrate level in waste water to be discharge after
treatment conforms to the standards.
5.2.1.1 Aims
To determining the nitrate concentration (mg/L NO3--N)
39
5.2.3 Methodology
Apparatus
DR 2000 spectrophotometer
Sample cell
Procedure
1. The stored program number for nitrate nitrogen was entered. The stored number is 355, then the
READ/ENTER key was pressed.
2. Wavelength dial was rotated until the displayed showed 500 nm.
3. The display showed mg/L N NO3- after the READ/ENTER was pressed.
4. The sample cell was filled with the filtered sample.
5. 1 pillow of the Nitra Ver 5 Nitrate reagent powder was added to the sample cell. The sample cell
was swirled to mix.
6. After pressing the button SHIFT then TIMER, the sample cell was shaken vigorously until the
beeped.
7. On pressing the button SHIFT then TIMER, 5 minutes reaction began.
8. When the timer beeped, a sample cell filled with sample (blank) was placed into the cell holder.
The light shield was closed.
9. The ZERO key was chosen.
10. The display showed WAIT then 0.0 mg/L N NO3-.
11. The sample cell containing the sample containing the Nitra Ver 5 Nitrate reagent was then placed
into the cell holder.
12. The reading was displayed in mg/L on pressing READ/ENTER.
13. The result was recorded.
5.2.3.1 Health and Safety Issues
Should wear gloves when handling the sample as the water used can be a vector of water-borne
diseases.
Should be careful when handling the powder pillow as its content is toxic.
40
Ion
Concentration
Nitrate
0.2 mg/L
5.2.5 Conclusion
The guideline value for nitrate in waste water is 10mg/L according to the Environment Protection Act
2002. Nitrate content in the sample is less than the threshold, so the sample does not require treatment to
decrease the level of nitrate in the water.
41
5.3 Phosphorus
Abstract
This practical involved the determination of the concentration of phosphorus in the wastewater sample.
The wastewater used for this part was initially filtered and diluted to a dilution factor of 5. The required
steps to use the spectrophotometer were followed and the concentration of phosphorus obtained was 9.7
mg/l PO42- which was below the acceptable limit.
5.3.1 Introduction
Phosphorus is an essential nutrient for plants and animals.
Groundwater rarely contain more than 0.1 mg/l phosphorus unless they have passed through solid
containing phosphate or have been diluted by organic matter.
Fertilisers and detergent are main sources of phosphorus compounds which are carried into surface as
well as groundwater in the form of sewage, industrial wastes and storm run-off. High concentrations of
phosphorus in water bodies may lead to accelerated plant growth, algae bloom, low dissolved oxygen and
hence death of fish and other aquatic beings.
The ascorbic acid method is used in this practical where orthophosphate reacts with molybdate in an acid
medium to produce a phosphomolybdate complex. Ascorbic acid then reduces the complex, giving an
intense molybdenum blue colour.
5.3.1.1 Aim
The main aim of this practical is to determine the phosphorus reactive concentration of the sample.
42
Since
wastewater is discharged into the sea after treatment, it should be ensured that the phosphorus level is within
acceptable limit because algae blooms can also be toxic and negatively impact swimming and fishing,
5.3.3 Methodology
Apparatus and reagents used
a) DR 2000 Spectrophotometer
b) Sample matching cells
c) PhosVer 3 Phosphate Powder Pillow
Procedure
1. To the sample of wastewater used for determination of phosphorus concentration, activated
charcoal was initially added and left to stand so as to clot the solid particles.
43
2. The sample was then filtered by applying suction, using the filtration apparatus as shown in the
picture below.
3. From the filtered sample, a test specimen of dilution factor 5 was prepared as follows: 20ml of the
wastewater sample was poured in a measuring cylinder and further topped up to the 100 ml mark
by addition of distilled water.
4. The stored program number for reactive phosphorus powder pillows was entered: 490. The
READ/ENTER button was pressed for units mg/l PO43-. The display showed: DIAL nm TO 890.
5. The wavelength dial was rotated until the small display showed: 890 nm.
6. The READ/ENTER button was pressed and the display showed: mg/l PO43- PV.
7. A sample cell was filled with 25 ml of the diluted sample of wastewater.
8. The contents of 1 Phos Ver 3 Phosphate Powder Pillow were added to the sample cell (the
prepared sample). The sample cell was swirled immediately to mix. A blue colour was seen
showing the presence of phosphate in the sample.
9. The SHIFT TIMER button was pressed after which a two minute reaction period started.
10. Another sample cell was filled with 25 ml of the diluted sample of wastewater (the blank).
11. The blank was placed into the cell holder and the light shield was closed.
44
12. After the timer had beeped, the display showed: mg/l P PV.
13. The ZERO button was pressed and the display showed: WAIT then: 0.00 mg/l PO43- PV.
14. The prepared sample was then placed into the cell holder and the light shield was closed.
15. The READ/ENTER button was pressed and the display showed: WAIT. Then the result in mg/l
PO43- was displayed and recorded.
5.3.3.1 Precaution
The sides of the sample cells were properly wiped with tissue paper to remove fingerprints left due to
handling.
References
1. YEOMAN, S., STEPHENSON, T., LESTER, J.N. AND PERRY, R., 1988. The removal of
phosphorus during wastewater treatment: A review. Environmental Pollution. 49 (3), 183-233.
45
5.4 Sulfate
Abstract
The concentration of sulfate ions in a water sample was determined during this experiment by the
turbidimetric method. Hence using a spectrophotometer, the amount of turbidity was related to the
amount of sulfate. Eventually, the concentration of sulfate in the water sample was displayed by the
spectrophotometer.
5.4.1 Introduction
Sulfate is an abundant ion and it is widely distributed in the nature. Sulfates may be present in natural
waters with concentration varying from a few hundred to several thousand mg/L. It is present in a large
number of minerals among which there are barite, epsomite and gypsum. Sulfates form salts with various
cations and these salts may be soluble or insoluble in water.
5.4.1.1 Aims
To determine the sulfate concentration (mg/L SO42-)
responsible for odour and corrosion of sewer systems which results from the conversion of sulfates into
hydrogen sulfide during reduction under anaerobic conditions. Estimation of the sulfate content of
wastewater can be important to the design engineer so that the latter can determine whether there is need
to provide for scrubbing facilities. Scrubbing facilities are used to remove the hydrogen sulfide at the
wastewater treatment plant.
Methods for sulfate removal from wastewater include:
Reverse osmosis
46
The maximum permissible limit of sulfate concentration in discharged wastewater is 750 mg/L (EPA
2002).
5.4.3 Methodology
5.4.3.1 Principle
The turbidimetric method is used for the determination of the sulfate concentration in water. The sulfate
ions in the water sample are reacted with barium in Sulfaver 4 Reagent to form a precipitate of barium
sulfate which causes turbidity. The concentration of sulfate ions in the water sample is proportional to the
turbidity formed.
Apparatus and Reagents
The equipment and reagents used are:
(a) DR 2000 Spectrophotometer
(b) Sample matching cells
(c) Sulfaver 4 Reagent Powder Pillow
Procedure
1. The stored program number for sulfate (SO42-) was entered. The number 6 0 8 was entered
and the READ/ENTER button was pressed. The display showed: DIAL nm TO 450.
2. The wavelength dial was rotated until the small display showed 450nm.
3. The READ/ENTER button was pressed. The display showed: mg/L SO42-.
4. A sample cell was filled with 25 ml of sample.
47
5. The contents of Sulfaver 4 Reagent Powder Pillow were added to the cell (the prepared
sample). The cell was then swirled to dissolve the reagent.
6. The SHIFT TIMER was pressed and a five minute reaction period began.
7. When the timer beeped, the display showed: mg/L SO42-.
8. Another sample cell was filled with 25 mL of sample (the blank).
9. The blank was placed into the cell holder and the light shield was closed.
10. Furthermore, the zero button was pressed. The display showed: WAIT and then 0.0 mg/L
SO42-.
11. Within five minutes after the timer beeped, the prepared sample was placed into the cell
holder.
12. The light shield was closed and READ/ENTER button was pressed. The display showed:
WAIT and then the result in mg/L SO42- was displayed.
5.4.3.2 Health and Safety
Handle the laboratory equipment with care to eliminate the risk of breaking equipment made of
glass and thus leading to injuries.
Avoid contact of the skin with the chemicals used by wearing safety gloves.
5.4.5 Discussion
The sulfate concentration of the wastewater sample is within the limit which has been set according to
Mauritius Environmental laws. The concentration of sulfate being 1 mg/L is below the maximum
permissible limit which is 750 mg/L. Therefore no treatment for sulfate is required for this wastewater
sample.
5.4.5.1 Limitations
Fingerprints on the sample cell affected the value of the reading obtained from the spectrophotometer.
48
5.4.6 Conclusion
It can be concluded that the wastewater sample provided has a concentration of sulfate that will not
adversely affect the sewage systems.
REFERENCES
1. Determination of sulfate concentration, 2014, (ONLINE). Available at:
http://nitttrc.ac.in/Four%20quadrant/eel/Quadrant%20-%201/exp9_pdf.pdf. Accessed on 29
March 2015.
2. Environmental engineering, Howard S Peavy, Donald r, Rowe George tchobanoglous, Mc Graw
Hill book company, Published in year 1985
3. Mohammed Sadeq Salman, Computer Centre/University of Baghdad. Removal of sulfate from
wastewater. [ONLINE] Available at: http://www.iasj.net/iasj?func=fulltext&aId=2357 Accessed
on 29th March 2015.
49
5.5 Chloride
5.5.1 Introduction
Chlorides are present in sewage as a metallic salt in the form of Cl - ions. Chlorides forms of one of the
major inorganic constituents in wastewater. Sources of chlorides includes the agricultural, industrial and
human wastewater. The chloride concentration in wastewater is higher than that in raw water since
chloride is a common ion found in all diets and passes unabsorbed by the body.
5.5.1.1 Aims and Objectives
The aim of this experiment is to determine the concentration of chloride anions present for the given
wastewater sample.
pollution. Chlorides are also leached from various rocks into the soil and finally into underwater
by weathering. Chlorides also protrudes into water from discharges of wastewater from
domestic, agricultural and industrial into surface water. Foe domestic wastewater, human waste
contain approximately 6g of chlorides per person per day (Metcalf & Eddy, 2003).
It is important to determine the amount of chloride in the effluent if the treated wastewater is
being reuse for irrigation and other agricultural purposes. Excess chloride has the tendency to
accumulate in soil tissues of some plant to toxic levels. When wastewater effluents containing
high amounts of effluents are discharged to the ground, the groundwater surrounding the disposal
site can result in high levels of sodium and chloride and thus leading to health problems.
50
5.5.3 Methodology
Apparatus:
Digital titrator
Conical flask
Measuring cylinder
Reagent:
Diphenylcarbazone
Digital titrator
Procedure:
1. The digital titrator was held with the tip pointing up. The delivery knob was turned to remove any
entrapped air and allow the flow of the titrant. The counter was set to zero and the tip was wiped.
2. 100 ml of sample was measured using a measuring cylinder and transferred to a conical flask.
3. One Diphenylcarbazone powder pillow was added and mixed.
4. The delivery tube tip was placed into the solution and the titrant was added drop by drop. While
titrating, the flask was swirled until a first colour change was observed.
5. The number of digits required for the colour change was recorded.
5.5.3.1 Health and Safety
Use of face mask and eye goggles to avoid inhaling of the Diphenylcarbazone powder pillow and
contamination of the eyes.
72
Colour change:
51
5.5.6 Discussion
Chloride reacts with mercuric nitrate to form soluble and slightly dissociated mercuric chloride. The
water sample was titrated under acidic conditions at pH 2.3 to 2.8 with diphenylcarbazone indicator. A
pink-purple complex is with the addition of excess mercuric ions
The Environment Protection Act, 2002 has established a guideline value of 750 mg/l for the maximum
allowable amount of chloride to be discharged in both land and surface water.
5.5.7 Conclusion
The wastewater can be discharge on land and in surface water since the standard limit for chloride content
as per the Environmental Protection Act have been met.
References
1. Apteand al., 2011, Chloride Removal from Wastewater by Biosorption with the Plant Biomass.
[Online]. Department of Environmental Science and Technology,Department of Technology,
Shivaji
University,
Kolhapur,
Maharashtra,
India.
Available
at:
52
6.0 pH
Abstract
The experiment consisted of dipping the electrode of a pH meter into a beaker containing the wastewater.
It was important to shake the wastewater in the gallon before pouring in the beaker in order to have a
uniform mix. The result has attributed the wastewater a pH slightly above neutral i.e. 7.
6.0.1 Introduction
The intensity of the acid or alkaline condition of a solution is expressed in terms of pH. It is a way of
expressing the hydrogen-ion concentration. The term pH refers to the measurement of hydrogen ion
activity in the solution. In wastewater treatment employing biological processes, pH must be controlled
within a range favourable to the particular organisms involved. Chemical processes used to coagulate
wastewaters, dewater sludges, or oxidise certain substances must be controlled within narrow limits
6.0.1.1 Aims
To determine the pH of the wastewater sample
53
6.0.3 Methodology
Apparatus
pH meter
250 ml Beaker
Test Procedure
1. Water was collected from the gallon and transferred it into a beaker.
2. pH meter was switched on.
3. The electrode was removed from storage solution and rinsed with water.
4. The pH electrode was dipped in the beaker containing the wastewater to be tested. The pH value
was recorded.
5. Finally, the electrode was rinsed with distilled water.
6.0.5 Conclusion
The pH of the wastewater sample is within limits (5-9) for effluent discharges specified in the regulations
made by the Minister under sections 39 and 96 of the Environment Protection Act 2002
54
Parameter
Obtained
values
EPA Discharge
Limits into Surface
water
BOD
COD
Suspended Solids
Settleable Solids
Ammonia
Nitrate
Phosphorus
Sulfate
Chloride
pH
26
179
125
2.8
35.4
0.2
9.7
1
7.2
7.3
40
120
35
not available
1
10
10
750
750
5 to 9
55
8.0 Appendix
8.0.1 Chloride Content
Figure 8.1: Digit multiplier for sample volume and Titration Cartridge (N Hg (NO3)2)
(Source: Adapted from Public Health Practical (water), Chloride, University of Mauritius, 2011)
56
57
Parameter
Unit
Surface
courses
Underground
Total coliforms
<400
ml
E. Coli
<200
ml
Free Chlorine
mg/l
0.5
45
35
Reactive Phosphorus
mg/l
10
mg/l
Colour
Not objectionable
Temperature
40
pH
59
mg/l
120
mg/l
40
Chloride
mg/l
750
Sulphate
mg/l
750
Sulphide
mg/l
0.002
Ammoniacal Nitrogen
mg/l
Nitrate as N
mg/l
10
mg/l
25
Nitrite as N
mg/l
58
water
Aluminium
mg/l
Arsenic
mg/l
0.1
Beryllium
mg/l
0.1
Boron
mg/l
0.75
Cadmium
mg/l
0.01
Cobalt
mg/l
0.05
Copper
mg/l
0.5
Iron
mg/l
2.0
Lead
mg/l
0.05
Lithium
mg/l
2.5
Manganese
mg/l
0.2
Mercury
mg/l
0.005
Molybdenum
mg/l
0.01
Nickel
mg/l
0.1
Selenium
mg/l
0.02
Sodium
mg/l
200
Total Chromium
mg/l
0.05
Vanadium
mg/l
0.1
Zinc
mg/l
mg/l
10
Total Pesticides
mg/l
0.025
mg/l
mg/l
0.1
Phenols
mg/l
0.5
mg/l
15
59
Date
25 March 2015
28 March 2015
2 April 2015
28 March 2015 to 6 April 2015
Activity
Wastewater Practical Session
Reporting of values obtained
Collection of results for BOD test
Compilation and editing of entire report
It is to be noted that all effective writings and other written works pertaining to the report was done as a
group and there were regular group meetings to evaluate the progress of the report.
8.0.3 Contribution of team members and resource persons
The different sections of this report have been discussed among team members. However, the structured
writing of each discussed section has been carried out by different members while field work such as
measurements of dimension from the building, were carried out by all team members. The following table
shows the contribution of each member during the writing process of the report.
Table 8.3: Contribution of team members
Section
Sub-section
Contributing member
LUBRUN Veeresh Kumar
Introduction
Biological and
chemical oxygen
demand
Test 1 BOD
Test 2 COD
Test 5Ammonia
BUNDHOO Akshay
KISTO Chusnee
BUNDHOO Akshay
LUBRUN Veeresh Kumar
AJODAH Trisha Ooshita Devi
HOW YUEN SIONG Yannick Van Pow
HOW YUEN SIONG Yannick Van Pow
KISTO Chusnee
Solids
Inorganic minerals
Test 6 Phosphorus
Test 7 Sulfate
Test 8 Chloride
Test 9 Nitrate
pH
General Conclusion
Overall Compilation of Report
60