ENVIRONMENTAL ENGINEERING TECHNOLOGY SECTION

UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

EXPERIMENT 1

JAR TESTING

1.0 INTRODUCTION

2.0 OBJECTIVE
i. To study relationship of heavy metal removal and pH

APPARATUS
1. 1 jar flocculate with pH adjustment

2. 6 graduated beakers (1L)

3. 2 of 10 mL graduated cylinders

4. 1 of 1000 mL graduated cylinders

5. 1 scale for weighing coagulants

6. 1 pH meter

7. 1 turbidity

3.0 REAGENT
1. Sample of waste water

2. 1% liquid Poly Aluminum Chloride (PAC) [refer chemical preparation]

3. 1% Sodium hydroxide* (NaOH) [refer chemical preparation]

4. 1% Sulfuric Acid* (H2SO4) [refer chemical preparation]

5. 0.1% An-Ionic Polymer[refer chemical preparation]

*Check pH sample. If pH <4 prepare NaOH. If pH >9 prepared H2SO4

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

4.0 PROCEDURE
1. 600 ml of waste water sample add into a 6 beakers and label as S1,S2,S3,S4,S5 & Ref

2. Measure the initial of pH, Turbidity, Zn, Mn & Cu

3. Fill burette with 1% H2SO4 or 1% NaOH (depend on sample). The initial burette reading is record

4. The H2SO4 or NaOH is added slowly from the burette into beakers and at the same time measure pH
of sample.

5. Record the addition of H2SO4 or NaOH is continued until the pH reach 4,5,6,7,8

6. Add 2 ml of 1% PAC into each sample S1-S5

7. Mix sample using jar test unit speed 200 rpm for 2 minutes

8. Add 2 ml of 0.1% Polymer into each sample

9. Mix slowly sample using jar test unit by reduce of speed to 50 rpm for 3 minutes

10. Wait for settle down of particle and measure the final of turbidity, Zn ,Mn & Cu each sample.

5.0 RESULTS

Table 1: The result reading for set 1 of Jar test.

Set 1
Jar Turbidity (FNU) Coagulation
Before After pH Dosage
experiment experiment (mL)
1
2
3
4
5
6 (Control)

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

Table 2: The result reading for set 2 of Jar test by using pH optimum.

Set 2
Jar Turbidity (FNU) Coagulation
Before After pH Dosage (mL)
experiment experiment (opt)

1
2
3
4
5
6 (Control)

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

EXPERIMENT 2

COAGULANT & FLOCCULENT TREATMENT PROCESS

1.0 OBJECTIVES

i. Understand the concept of coagulation, flocculation and settling.

ii. Obtain the optimum flow rates of coagulant and flocculants for the coagulation -
flocculation process.
iii. To analysis efficiency of turbidity reduction

2.0 METHOD
Non standard method

3.0 APPARATUS
1. Die powder/ waste water
2. Tap water
3. Beaker
5. pH meter.
6. Turbidity meter.
4.0 REAGENT
1. Preparation of sample dilute with die / waste water
2. 5 L of 1% PAC or Alum fro 5 L fill in Coagulant Tank
3. 3 L of 0.1 % of Polymer and fill in Flooculant Tank
4. 3 L of 1% of NaOH (Prepare in proper container)
[Please refer the formula table and chemical preparation]

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

5.0 PROCEDURE

5.1 GENERAL START-UP PROCEDURE

1. Drained the feeding tank D1

2. Drained the settler D4
3. The plastic hose was connected through to the feeding pump G2
4. The electrical connections was carried out to the pump G1
5. Closed the Valve V1 and V9
6. Closed the valve V4 of the reactor R1
7. Closed the valve V6 of the reactor R2
8. Closed the valve V8 of the reactor D4

EXPERIMENT PROCEDURE
1. Switch on the power supply. The automatic or differential switch was connected and
the START button was press, the plan is ready for manipulation
2. Fill the tank D1 with the 200L wastewater sample to be treated [refer to the
technician]
3. Switch pump G1 to 1 for mix of sample wastewater
4. Fill the tank D2 with the solution 5L of 1% of alum or PAC
5. Fill the tank D3 with the solution 500 ml of 0.1% of POLYMER
6. Start the pump G2, switch to 1
7. Set the flow rate [ Q ] 100 L/hr
8. Wait until ½ of sample in tank R1, Start the motor M1, switch to 1 & motor 2 will start
automatically.
9. Start the pump G3, switch to 1
10. Set the flow rate FI3 .Flow rate base on calculation DOSE of alum or 1% PAC.
11. Control the pH of sample in R1 to optimum pH [refer on data from Jar Test Experiment
in Table 1].pH will drop when sample mix with PAC or Alum.
12. Control pH to optimum pH by add 1% of NaOH manually.

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

13. Sample from R1 will over flow to R3 tank

14. Wait until ½ sample in tank R3 ,on the pump G4
15. Set the % flow rate of DOSE of 0.1% Polymer
16. Sample treated over flow to sedimentation tank D4
17. Wait until all process are complete and measure turbidity D1,D2,D3 & D4

5.2 SHUTDOWN
1. After experiment complete, switch off all the pump, motor & switch off main power
2. Open all valve to remove sample / solution from the tank
3. Clean all the tank D1,D2,D3 ,D4,R1,R2 & R3

6.0 RESULT

Initial turbidity [NTU]

Initial pH [ / ]

Final turbidity [ NTUf ]

Final pHf [ / ]

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

Data from Jar Test:

Optimum pH [ / ]

Optimum coagulant (PAC) dosage [mg/L]

Optimum flocculent (Polymer) dosage [mg/L]

[ Technician will provide]

Analysis Question:

1) Draw Process Flow Diagram (PFD) and explain coagulation, flocculation and settling
process?
2) Explain detail factor in determining efficiency of turbidity reduction?
3) Explain source of error that might happen in this experiment?

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

EXPERIMENT 3:

WASTEWATER QUALITY DETECTION OF HEAVY METALS ( AAS )

7.0 OBJECTIVE

1. To determine the concentration of Lead (Pb),Copper (Co) and Zinc(Zn) in waste water
sample using AAS as common method of heavy metal detection

8.0 METHOD

The concentration of an element in solution is determined by measuring the quantity of light

of specific wavelength absorbed by atoms of the elements released in a flame. Figure 9.1
shows an atomic absorption spectrophotometer, which consist of an atomizer-burner to
convert the element in solution to free atoms in an air acetylene flame. This is followed by a
monochromator (prism and slit) to disperse and isolate the light waves emitted, and a
photomultiplier to detect and amplify the light passing through the monochromator. The light

source is a lamp with a cathode formed of the same element being determined, since each
element has characteristic wavelengths that are readily absorbed.

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

The light passing through the sample is separated in the monochromator into its component
wavelength. The photomultiplier then receives only the isolated resonance wavelength. The
amount of energy at the characteristic wavelength absorbed in the flame is proportional to
the concentration of the element in the sample.

9.0 APPARATUS
9 100mL volumetric flask with cap
1 250mL beaker
1 Dropper
AAS (Atomic Absorption Spectrophotometer) using air
1 Acetylene flame for Pb, Co & Fe determination
1 AAS (Atomic Absorption Spectrophotometer with graphite furnace)
And using argon hydrogen air flame for As determination

Note: This is a demo session only. Laboratory technician will perform this experiment but
you are required to prepare the standards for the calibration curve. Three groups will share
preparing the standards, blank and one water sample.

10.0 REAGENT
1000mg/L Pb stock solution
1000mg/L Fe stock solution
1000mg/L Fe stock solution
65% concentrated Nitric Acid (HNO3)

11.0 PROCEDURE

Preparation of standard 100mg/L from stock solution 1000mg/L Pb /Co/Zn

1. The stock solution is first diluted to become 100mg/L by transferring 10mL of 1000mg/L
into 100mL capacity volumetric flask.

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

2. Add 10 drop HNO3 (65% Concentrated)

3. Then add distilled water to the mark
4. The flask is then inverted several times to mix the contents properly.

Preparation of standards new stock solution for Pb /Co/Zn from 100mg/L

Calculate the amount required to obtain 1.0, 2.0 and 3.0 mg/L standard solution for
Pb/Fe/Zn from 100mg/L new stock solution. Example calculation: To prepare 0.5mg/L
Pb/As/Zn.

x
*100mg/L  0.5mg/L
100
where, x is the amount of standard required
100 is the capacity of volumetri c flask used
100mg/L is the new stock solution
0.5mg/L standard solution required to prepare
Therefore, x is 0.5mL

Preparation new stock solution for Pb /Co/Zn from 100mg/L

1. Pipette 0.5mL of 100mg/L stock solution

2. Place in 100mL volumetric flask
3. Add distilled water until the mark
4. Add 10 drops of con. HNO3. Please carry out this step at the fume cupboard.
5. Mix the contents by inverting the flask several times.
6. Repeat the same steps (1- 5) for preparing 1 mg/L, 2 mg/L and 3 mg/L standard
solutions.
7. For 0 mg/L or blank, use 100mL distilled water instead and add 10 drops of HNO 3.
8. For the sample, place 100mL of water sample in 100mL volumetric flask and then add 10
drops of con. HNO3

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

9. After preparation for sample, standards and blanks has completed, the technician will
operate the AAS, plot the standard curve and measure the concentration of Pb , Zn and
As for you

Preparation of sample
1. Prepared 50 ml of sample
2. Add 10 ml of 65% HNO3 and heat slowly until boil
3. Add another 10 ml of 65% HNO3
4. Make sure color of sample are clear
5. Add 5 ml 37% of HCl
6. Transfer sample to 50 ml of volumetric flask
7. Dilute with DI water until mark and sample ready to analyse using AAS
*All preparation & digestion, please use fume hood and use goggle and proper glove

12.0 RESULT

Heavy Metal Concentration of heavy metal

[ppm]
Pb
Co
Zn
Initial pH [ pHi ]

13.0 Analysis Question:

1. Analyse relationship of heavy metal concentration corresponding to the initial pH of
waste water?
2. Compare result with parameters limits of heavy metal in effluent as IER 2009.

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LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

EXPERIMENT 4

OIL & WATER SEPARATOR

1.0 INTRODUCTION

The Oil Water Separator (Model: BP 13) has been designed to demonstrate the basic
principles of a liquid-liquid separation process based on density differences. The normal
mode of operation is that two immiscible liquids with different densities such as oil and
water are pumped into a mixing chamber. Agitation of the two phases in the mixing
chamber will cause an emulsion to form between the two liquids. The emulsion mixture
will then flow into the settling chamber where they are settled and separated again into
two different light and heavy phases.

The separation efficiency can be affected by the residence time in the separator and
also the mixture composition. The effect of residence time can be studied by varying the
flow rates of both light and heavy phase, while the effect of mixture composition can be
observed by varying the flow rate ratio of the two different phases.

Sample points are provided at the plant to allow for collection of both light and heavy
phase liquid. Composition analysis of the final separated phases can then be carried out
by measuring the liquid’s density and comparing with a prepared calibration curve.

A process flow diagram of the plant is shown in Figure 1.

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

(Water)
V3

B1

V13
V1
P1
P2

V2

Figure 1. Single Stage Mixer Settler Process Diagram.

V14
MIXER SETTLER
SINGLE STAGE

V4

(Oil)
B2
sampling
V10

V12
V8
V7

V11
sampling
V9

(EXTRACT)
B4

V16
V6

(RAFFINATE)
B3

V15
V5

Figure 1: Process Flow Diagram for the Oil Water Separator

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

OBJECTIVE:

To operate a liquid-liquid separation experiment using a single stage mixer

settler.

To determine the effect of residence time on the separation efficiency.

PROCEDURES:

1. Ensure that the calibration data for density vs. composition of oil-water
mixtures are obtained.

2. Perform the start-up procedures as outllined in Section 3.2.

3. Open valves V1 and V2. Switch on the pumps P1 and P2.

4. Set both oil and water flow rates at 5 L/hr each by adjusting the pumps’
settings.

5. Let the experiment run for a while to attain steady state.

6. At steady state, collect samples as follows:

a) Sample at valve V11 and label as separated water (heavy phase)

b) Sample at valve V12 and label as separated oil (light phase)

7. Measure the density of both samples and use the prepared calibration curve
to determine the remaining oil or water composition in each sample.

8. Repeat the experiment (steps 4 to 7) by increasing the flow rates of both oil
and water to 10, 15 and 20 L/hr each. Make sure that both flow rates are the
same.

9. Record all data in the table in Appendix B.

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LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

ANALYSIS AND DISCUSSION:

1. Calculate the separation efficiency for each experiment as follows:

Amount of oil in separated water

Efficiency = 1
Amount of oil entering the mixer settler

2. Compare and comment on the efficiency at different residence times.

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UniKL MICET
LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

EXPERIMENT 5

AEROBIC UNIT

1.0 Objective

To measure the efficiency of aerobic processes by calculating the percentage of reduction of COD
of the wastewater effluent at different time interval.

2.0 Concept

Aerobic digestion of waste is the natural biological degradation and purification process in which
bacteria that thrive in oxygen-rich environments break down and digest the waste. Of all the biological
treatment methods, aerobic digestion is the most widespread process that is used throughout the world.

3.0 Apparatus

Aerobic Unit

pH meter

COD Analyzer

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LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

4.0 Procedure

1. prepare sample- 292 ml methanol+ 700 L H2O

2. add R1 with sample until 10 cm under overflow pipe
3. on compressor (600 NL/H) and stirrer
4. turn on the selector manual
5. set feed flow rate to 20L/H, and recycle to 15L/H
6. turn on the selector to auto
7. press reset
8. add activated sludge into R1
9. 30 ml sodium hypochlorite into D4 and DW
10. Add D2 and D3 with water
11. Connect the tank of the water to be treated, to the pump G1
12. Conduct the COD analysis at the outlet after approximately 2 days of operation of the
plant

5.0 Observation

Initial

COD concentration :………………..mg/l

pH:……………….

Temperature :………………….

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LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

Time interval COD concentration (mg/l) % reduction

After 8hr operation

After 16hr operation

After 24hr operation

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LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

EXPERIMENT 6

ANAEROBIC UNIT

1.0 Objective

To measure the efficiency of anaerobic processes by calculating the percentage of reduction of

COD of the wastewater effluent at different time interval.

2.0 Concept

The goals of anaerobic digesters are to biologically destroyed a significant portion of the volatile
solids in sludge and to minimize the putrescibility (decomposition of plants and animals after death
resulting in the production of unpleasant substances) of sludge. The main products of anaerobic digesters
are biogas and not harmful digested sludge solids. Biogas consists mostly of methane (CH4) and carbon
dioxide (CO2).

3.0 Apparatus

Anaerobic Unit

pH meter

COD analyzer

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LAB MANUAL WASTE WATER TREATMENT TECHNOLOGY (SEPT 2015)

4.0 Procedure

1. Prepare four packet of sugar and 1500g of Biolen and dissolve it in water.
2. Fill the tank until it full in 7 litre and mix it with dissolve of sugar and Biolen.
3. Start up the procedure to run the experiment.
4. Take the first sample and analysis the COD.
5. Analysis the COD everyday until six days and also take the pH and temperature reading.
6. After finish, shut down.

5.0 Observation

Initial

COD concentration :……………mg/l

pH :…………..

Temperature :……………..

Dy pH Temperature COD reading % reduction

mg/l

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