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NKB 31102

CHEMICAL ENGINEERING LABORATORY 3

PRE-LAB PROPOSAL
LAB 25
ENVIRONMENTAL SCIENCE

GROUP MEMBERS:
AMEERUL AFIQ BIN ABD HALIM 55220218047
ARINA HAZIRAH BINTI ZULKEFLI 55220116087
MOHD ASRAF BIN MOHD SAID 55220217088
YUWETA D/O GUNASAGRAN 55220217169

LECTURER:
MADAM RUSMAWARNI RAMLI
Objective

• To study the qualitative and quantitative value of waste water sample of Taman Jati Indah, Alor
Gajah
• To evaluate and compare the analysis result with the Malaysia Environmental Quality Act 1974,
(Sewage) Regulation 2009

Introduction

pH is a way of expressing the hydrogen-ion concentration of a solution. As acids and bases in


solution dissociate to yield hydrogen ions [H+] and hydroxyl ions [OH-] respectively, pH is used to indicate
the intensity of the acidic or alkaline condition of a solution. pH is key water quality parameters in
environmental engineering practice. In the water supply and treatment fields, these parameters have
great influence on the chemical coagulation, disinfection and softening processes, and corrosion control
for water distribution pipe networks (Ntwampe &d Jewell & Hildebrandt, 2003). Effective chemical
coagulation of water, for instance, occurs only within a specific pH range. Chemicals used for coagulation
release, as a by-product of their reactions with water to form insoluble hydroxide precipitates, hydrogen
ions (acid-causing). If unchecked, these hydrogen ions could lower the pH of the water sufficiently to
render the coagulants ineffective. The presence of a sufficient amount of alkalinity in the water can react
and remove the hydrogen ions released by the coagulants, thus buffering the water in the pH range where
the coagulant can be effective. In pure water, water molecules dissociate into equal amounts of hydrogen
and hydroxyl ions (10-7 moles/L). From the law of mass action, it can be shown that for pure water at
about 25°C:
[H+] x [OH-] = KW = 10-14………. (1)

The pH value of a solution has been defined to be the negative log of the hydrogen ion
concentration:
pH = -log[H+]………… (2)

The pH scale runs from 0 to 14, with pH 7 representing neutrality. Acid conditions increase as
pH values decrease, and alkaline (base) conditions increase as the pH values increase. Measurement
of the hydrogen ion concentration is made by pH meters via a glass electrode and a calomel reference
electrode.

Turbidity is the technical term referring to the cloudiness of a solution and it is a qualitative
characteristic which is imparted by solid particles obstructing the transmittance of light through a water
sample. Turbidity often indicates the presence of dispersed and suspended solids like clay, organic
matter, silt, algae and other microorganisms. When the turbid water in a small, transparent container such
as drinking glass is held up to the light, an aesthetically displeasing opaqueness or milky colouration is
apparent. The colloidal material which exerts turbidity provides adsorption sites for chemicals and for
biological organisms that may not be harmful. They may be harmful or cause undesirable tastes and
odours. Disinfection of turbid water is difficult because of the adsorptive characteristics of some colloids
and because the solids may partially shield organisms from disinfectant. Knowledge of the turbidity
variation in raw water supplies is useful to determine whether a supply requires special treatment by
chemical coagulation and filtration before it may be used for public water supply (Murugesan &
Rajakumari, 2005). Turbidity measurement is used to determine the effectiveness of treatment produced
with different chemicals and the dosages needed. Turbidity measurements help to gauge the number of
chemicals needed from the day-to-day operation of water treatment works. Turbidity measurements are
useful to determine the optimum dosage of coagulants to treat domestic and industrial wastewaters.
Turbidity determination is used to evaluate the performance of water treatment plants. Turbidity is based
on the comparison of the intensity of light scattered by the sample under defined conditions with the
intensity of light scattered by a standard reference suspension under the same conditions. The turbidity
of the sample is thus measured from the amount of the light scattered by the sample taking a reference
with standard turbidity suspension. The higher the intensity of scattered light the higher is turbidity.
Turbidity measurements performed using proprietary nephelometric instruments are expressed as
Nephelometric Turbidity Units (NTU) (Altaher & Alghamdi,2011). The nephelometric apparatus is
designed to measure forward scattering of light at 90° to the path of an incandescent light beam.
Suspended particles present in a water sample reflect a portion of the incident light off the particle surface.
The light reflected at 90° is measured by a photoelectric detector and is compared against light reflected
by a reference standard. No interference exists for the turbidity test.

Dissolved solids refer to any salts, minerals metals, or ions dissolved in water while suspended
solids refers to small solid particles which remain in suspension in water as a colloid or due to the motion
of the water. By standard measurement, any particles larger than 2 microns in water are considered
suspended solid while anything smaller than 2 microns are dissolved solids. High levels of suspended
solids have shown to increase water temperatures due to the fact that suspended solids are more heat
absorbent than water molecules. Warmer water holds less oxygen than its cold counterpart, thus reducing
the dissolved oxygen (DO) level in the water (Murphy, 2007).

Biochemical Oxygen Demand (BOD) is a chemical procedure done to determine how fast
biological organisms use up oxygen in water. These organisms exert oxygen demand as they try to
stabilize themselves during the decomposing process in which they convert nitrogenous compounds to
more stable forms. Hence, part of the oxygen demand is measured in the BOD process (Pennsylvania
Department of Environmental Protection, n. d). BOD is used in water quality assessment and
management, environmental science and ecology. Higher amount of organic matter will lead to higher
BOD, which correlates to reduced amount of dissolved oxygen available for animals such as fishes.
Therefore, BOD is a reliable gauge for indicating water pollution (Curley, 2010). This method is commonly
expressed in milligrams of oxygen consumed per litre of sample during 5 days of incubation at 20°C.
However, this leads to a disadvantage as it would take such a long time to obtain the result for the BOD.
Nowadays, BOD can be executed by reducing the days of incubation to 3 days and at 27°C since the
result will be equivalent to 5 days BOD at 20°C (Envis, n. d).

Measurement of COD can be made on samples of waste water of natural waters contaminated
by domestic or industrial waste. Chemical oxygen demand is in which a closed water sample is incubated
with a strong chemical oxidant under specific conditions of temperature and for a particular period of time.
(Camlab, 2009). Since nearly all organic compound is oxidized in the COD test, thus COD always higher
than BOD as BOD only decompose some of organic. Standard test for COD is using a mixture of
potassium dichromate and sulphuric acid to oxidize organic matter with silver added as catalyst.
COD is involving process of oxidation. As this process complete, the concentration of organics in
the sample is calculated by measuring the amount of oxidant remaining in the solution. This is usually
done by titration, using an indicator solution. COD is expressed in mg/L, which indicates the mass of
oxygen consumed per litre of solution. COD test only takes a few hours to get the result.
(Merckmillipore,n.d)
Experimental Procedure

Study 1: pH

Materials
• Sample
• Ph meter
• Buffer solution (4 and 9)

Procedure
1. Warming up the instrument for 15 minutes before use. Adjusted the pH knob to read 7 and
carefully connecting the electrode with the pH meter.
2. Washed the electrode in distilled water, wiped it dry and then immersed it in the buffer solution
(4.0).
3. Adjust the temperature knob to the temperature range of the buffer. Similarly, adjust the buffer
knob to the pH of the buffer solution, i.e.4.
4. Now turn the selector switch to zero position. Washing the electrode with distilled water, wiped it
dry and immersed it in the buffer solution of pH 9.2 and dipped the electrode in the sample.
5. According to the pH range of the sample, adjust the selector switch to either 0-7 or 7-14. Read
the pH of the sample.
6. Remove the sample; shift the selector switch again to zero position. Put off the instrument. Always
kept the electrodes dipped in distilled water.

Study 2: Turbidity

Materials
• Turbidity meter
• Sample
• Standard flask
• Funnel
• Wash bottle
• Tissue paper
• Hexamethylenetetramine
• Hydrazine sulphate
• Distilled water

Procedure

For testing the given water sample first the reagents are to be prepared. Then the turbidity meter is
required to be calibrated.

Preparation of reagents
Hydrazine Sulphate
1. Weigh accurately 1 g of hydrazine sulphate and dissolve it in turbidity-free distilled water.
2. Take 100 ml standard measuring flask and place a funnel over it.
3. Transfer it to a 100 ml standard flask and makeup to 100 ml using turbidity-free distilled water.
Hexamethylene Tetramine
1. Weigh accurately 10 g of Hexamethylenetetramine and dissolve it in turbidity-free distilled
water.
2. Take 100 ml standard measuring flask and place a funnel over it.
3. Transfer it to a 100 ml standard flask and makeup to 100 ml using turbidity-free distilled water
Standard 4000 NTU Solution
1. Mix 5 ml of hydrazine sulphate solution and 5 ml of Hexamethylenetetramine solution in a 100
ml standard measuring flask.
2. Allow the mixture to stand for 24 hours.
3. After 24 hours, make up the volume to 100 ml using turbidity-free distilled water.
4. The standard 4000 NTU solution is ready.

Calibration of turbidity meter


1. Using the standard solution calibrate the instrument.
2. The instrument is having four knobs, out of which the two knobs in the bottom is the set zero knob,
this is for setting the instrument to zero.
3. The one which is there in the top left-hand side is the calibration knob, used for the calibration.
4. The other one in the top is the knob for setting the detection range. It is adjusted to 1000 NTU
range.
5. To the sample cells, add turbidity-free distilled water up to the horizontal mark, wipe gently with
soft tissue.
6. Place it in the turbidity meter such that the vertical mark in the sample cell should coincide with
the mark in the turbidity meter and cover the sample cell.
7. Now using the set zero knob, adjust the reading to zero.
8. According to our need, prepare a standard solution. In this case, a 200 NTU solution is prepared
by diluting the standard 4000 NTU solution and added to the sample cells, up to the horizontal
mark, wipe gently with soft tissue.
9. Place it in the turbidity meter such that the vertical mark in the sample cell should coincide with
the mark in the turbidity meter and cover the sample cell.
10. If the instrument is not showing 200 NTU, using the calibration knob adjust the reading to 200
NTU.
11. Repeat the procedure for two / three times. Now the instrument is calibrated

Testing of water sample


1. To the sample cells, add sample water up to the horizontal mark, wipe gently with soft tissue and
place it in the turbidity meter such that the vertical mark in the sample cell should coincide with
the mark in the turbidity meter and cover the sample cell.
2. Check for the reading in the turbidity meter. Wait until you get a stable reading.

Study 3: Total Dissolved Solids and Total Suspended Solids

Apparatus
• Analytical Balance
• Crucible
• Vacuum Pump
• Filter Flask
• Desiccator
• Drying Oven
• Evaporating Disc
• Measuring Cylinder
• Forceps
• Pipette
Material
• Whattman Filter Paper
• Water sample

Procedure
The initial weight of a crucible, and an evaporating dish with a whattman filter paper are
measured by using an analytical balance. The readings are recorded as the dry weight of the items.
Measure 100 ml of water sample by using a measuring cylinder, and pour the content into the filter
flask. Place the weighed whattman filter paper to the end of the filter tip tighten the filter. When the
setup is secured, the vacuum pump connected to the filter flask is turned on. After 50 ml of water
sample has been filtered, the vacuum pump is turned off. Carefully remove the top filter to secure the
used whattman filter paper. Measure 20 ml of the filtered water sample into the weighed crucible by
using a pipette and place the used whattman filter paper into an evaporating dish. Both the filtered-
water-sample-containing crucible and used-whattman-filter-paper-containing evaporating dish are
placed into an oven. The oven is turned up to 103°C for about 1 to 2 hours, until the samples are
completely dried. The dried crucible and evaporating dish are then cooled to room temperature inside
the desiccator. The crucible and evaporating dish are weighed again using the analytical balance. The
readings are recorded as the final weigh of the crucible and evaporating dish.

Study 4: COD

Apparatus
• 500 ml Erlenmeyer flask
• Burette
• Glass rod

Material
• Standard potassium dichromate solution
• Concentrated sulphuric acid
• Silver sulphate
• Standard ferrous ammonium sulfate
• Standard dichromate solution
• Mercuric sulfate: Powdered hgso4
• Phenanthroline ferrous sulfate indicator solution

Procedure
Preparation of reflux mixture
1. Pipette a 50.0 ml aliquot of sample not to exceed 800 mg/L of COD into a 500 ml,flat bottom,
Erlenmeyer flask.
2. Add hgso4 in the ratio of 10 mg to 1 mg chloride, based upon the mg of chloride in the sample
aliquot and 5 ml of sulphuric acid.
3. Swirl until all the mercuric sulphate has dissolved.
4. Add 25.0 ml of 0.25M K2Cr2O7.
5. Carefully add 70 ml of sulphuric acid-silver sulphate solution and gently swirl until the solution
is thoroughly mixed.
6. Glass beads should be added to the reflux mixture to prevent bumping, which can be severe
and dangerous.
7. Cool, and wash down the interior of the condenser with 25 ml of distilled water. Disconnect the
condenser and wash the flask and condenser joint with 25 ml of distilled water so that the total
volume is 350 ml. Cool to room temperature
Caution: The reflux mixture must be thoroughly mixed before heat is applied. If this is not done, local
heating occurs in the bottom of the flask, and the mixture may be blown out of the condenser.

Titration
1. Titrate with standard ferrous ammonium sulfate using 10 drops of ferroin indicator. (The color
change is sharp, going from blue-green to reddish-brown and should be taken as the end point
although the blue-green color may reappear within minutes).
2. Run a blank, using 50 ml of distilled water in place of the sample together with all reagents and
subsequent treatment.
3. For COD values greater than 800 mg/L, a smaller aliquot of sample is took; however, the
volume should be readjusted to 50 ml with distilled water having a chloride concentration equal
to the sample.
4. Chloride correction (1): Prepare a standard curve of COD versus mg/L of chloride, using sodium
chloride solutions of varying concentrations following exactly the procedure outlined. The
chloride interval, as a minimum should be 4000 mg/L up to 20,000 mg/L chloride. Lesser
intervals of greater concentrations must be run as per the requirements of the data, but in no
case must extrapolation be used.

Study 5: BOD 3 days

Apparatus:
1. 4 x 300ml bottles having a ground glass stopper and flared mouth
2. Water bath or incubator

Procedure:

Reagent preparation
1. Phosphate buffer solution:
Dissolve 8.5 g KH2PO4, 21.75 g K2HPO4, 33.4 g Na2HPO4 7H2O, and 1.7 g NH4Cl in about
500 ml distilled water and dilute to 1 L. The ph should be 7.2 without further adjustment.
2. Magnesium sulphate solution:
Dissolve 22.5 g mgso4.7H2O in distilled water and dilute to I L.
3. Calcium chloride solution:
Dissolve 27.5 g cacl2 in distilled water and dilute to 1 L.
4. Ferric chloride solution:
Dissolve 0.25 g fecl3 6H2O in distilled water and dilute to 1 L.
Acid - While stirring, slowly add 28 ml concentrated sulphuric acid (H2SO4) to distilled water.
Dilute to 1 L.
Alkali - Dissolve 40 g sodium hydroxide (naoh) in distilled water. Dilute to 1 L.
5. Nitrification inhibitor, 22-chloro-6-(trichloromethyl) pyridine
6. Dilution water:
Use demineralised, distilled, tap, or natural water for making sample dilutions.

* Reagents are prepared by laboratory technician.

Sample pre-treatment

pH samples were checked before testing.


1. Samples containing caustic alkalinity (pH > 8.5) or acidity (pH < 6.0) will be neutralized samples
to pH 6.5 to 7.5 with a solution of H2SO4 or NaOH.
2. Sample temperature adjustment - Bring samples to 20°C - 21°C before making dilutions.
3. Nitrification inhibition - 3 mg of 2-chloro-6-(trichloromethyl) pyridine (TCMP) will be added to each
300 ml bottle before capping.

Sample dilution technique


1. Dilutions will be prepared either in graduated cylinders or volumetric glassware, and then transfer
to BOD bottles or prepare directly in BOD bottles.

DO and BOD Test


1. Water sample will be diluted.
2. Since the waste water source is from Taman Jati Indah, the sample will be diluted from 1 to 5%
(for raw and settled wastewater)
3. Sample pre-treatment and sample dilution will be carried out.
4. 3 bottles will be prepared.
5. 2 bottles with original (or diluted, inhibited) and diluted samples will be filled up and the last one
with control to the brim of the bottles.
Bottle 1 - original sample (or diluted, inhibited) (t = 0 and 3 days)
Bottle 2 - diluted sample (t = 0 and 3 days)
Bottle 3 - control sample (t = 0 and 3 days)
6. The control bottle should contain only the dilution water.
7. Initial DO concentration will be determined by using the DO probe for the diluted samples (in
duplicate) and control sample.
8. Stopper the bottles tightly, water seal and incubate for 3 days at room temperature. After 3 days
incubation determine the final DO in diluted sample and control.
Result

Study 1: pH

Sample Time(min) pH The volume of titration


(ml)

Study 2: Turbidity

The temperature of Sample


Sample No. (ºC) Time (min) Turbidity (NTU)

1.

2.

3.

Study 3: Total Dissolved Solids and Total Suspended Solids

Description Value
1 Weight of dry crucible, g, W 1
2 Weight of Evaporating dish and whattman filter
paper, g, W 2
3 Final weight of crucible, g, W 3
4 Final weight of evaporating dish and residue, g, W 4
5 Volume of sample, ml, V

Study 4: COD

Type of sample COD(mg/L)

Blank

Sample 1

Sample 2

Study 5: Biological Oxygen Demand 3 (BOD3)

Non-diluted sample.
Sample DO before incubate DO after Incubate (mg/l) BOD calculations (mg/l)
(mg/l)
Control
1

Diluted sample.
Sample DO before incubate DO after Incubate (mg/l) BOD calculations
(mg/l) (mg/l)
Control
1

Reference

Aik Heng Lee and Hamid Nikraz. (2015). BOD: COD Ratio as an Indicator for River Pollution. International
Proceedings of Chemical, Biological and Environmental Engineering, Vol. 88
A.G Murugesan and C Rajakumari (2005), Environmental Science and Biotechnology, Theory and
Techniques, MJP Pub. Chennai, pp. 127-132.
Camlab. (2009, October 16). COD or Chemical Oxygen Demand definition. Retrieved from
https://camblab.info/wp/index.php/272/
Curley, Robert. (2010). Biochemical oxygen demand (BOD). Retrieved from
https://www.britannica.com/science/biochemical-oxygen-demand
Envis. (n. d). Biochemical Oxygen Demand (BOD). Retrieved from
http://www.envis.org/EnvAnalysis/HtmlFiles/B/BiochemicalOxygenDemand.htm
H Altaher and A Alghamdi (2011), Enhancement of Quality of Secondary Industrial Wastewater Effluent
by Coagulation Process: A Case Study. Journal of Environmental Protection, 2011,2,1250-1256.
I.O Ntwampe, L L Jewell, D Hildebrandt and D Glasser (2013), The effect of water hardness on paint
wastewater treatment by coagulation-flocculation Journal of Environmental Chemistry and
Ecotoxicology Vol. 5(3), pp. 47-56.
Merckmillipore. (n.d). Water for COD - Chemical Oxygen Demand. Retrieved from
https://www.merckmillipore.com/MY/en/water-purification/learning-centers/applications/environment-
water-
analysis/cod/CLqb.qB.BIMAAAFAZwsQWTdi,nav?ReferrerURL=https%3A%2F%2Fwww.google.com
%2F&bd=1
Murphy, Shiela. (2007). General Information of Solids. Retrieved March 1, 2019, from
http://bcn.boulder.co.us/basin/data/NEW/info/TSS.html
Pennsylvania Department of Environmental Protection. (n. d). Chapter 5: Biochemical Oxygen Demand
(BOD). Retrieved from https://www.watereducation.org/sites/main/files/file-
attachments/pennsylvania_department_of_environmental_protection_biochemical_oxygen_demand.
doc
Statista. (2017). Distribution of rivers in Malaysia in 2017, by water quality. Retrieved from
https://www.statista.com/statistics/796339/share-of-rivers-by-water-quality-malaysia/
Turbidity, Total Suspended Solids & Water Clarity. (n.d.). Retrieved March 1, 2019, from
https://www.fondriest.com/environmental-measurements/parameters/water-quality/turbidity-total-
suspended-solids-water-clarity/
Appendix

Total Dissolved Solid Calculation

𝑊3 − 𝑊1 1000𝑚𝑔
𝐶1 = ∗
𝑉 1𝑔

Total Suspended Solid Calculation

𝑊4 − 𝑊2 1000𝑚𝑔
𝐶2 = ∗
𝑉 1𝑔
COD Calculation

𝑚𝑔 [(𝐴 − 𝐵)𝐶 ∗ 8000] − 50𝐷


𝐶𝑂𝐷 = ∗ 1.2
𝐿 𝑚𝑙 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
where:
A = mL Fe(NH4)2(SO4)2 for blank;
B = mL Fe(NH4)2(SO4)2 for sample;
C = normality of Fe(NH4)2(SO4)2;
D = chloride correction from curve
1.2 = compensation factor to account for the extent of chloride oxidation which is dissimilar in systems
containing organic and non-organic material.

BOD Calculation

𝐵𝑂𝐷3 = [(𝑎 − 𝑏) – (𝑐 − 𝑑)] ∗ 𝑛


Where:
a = DO sample before incubation
b = DO sample after 3 days of incubation
c = DO of control before incubation
d = DO of control after incubation
𝑚𝑙 𝑠𝑎𝑚𝑝𝑙𝑒 + 𝑚𝑙 𝐷𝐼 𝑤𝑎𝑡𝑒𝑟
n = Dilution factor, 𝑚𝑙 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒