Lab Manual Ieee

ENVIRONMENTAL ENGINEERING
LAB MANUAL
DEPARTMENT OF CIVIL ENGINEERING,

FAST-NU, LAHORE
Lab Manual of Environmental Engineering
Created by: Engr. Ali Zulqarnain

Date: 15th December, 2014
Last Updated by: Engr. Rizwan Amjad

Date: 19th July, 2016
Approved by the HoD: Dr. Shahid Ali

Date: 01th Aug, 2016
Page | 2
Table of Contents
Sr. No. Description Page No.
1 List of Equipment 5
2 Experiment No. 1, Determination of pH of water sample 6
3 Experiment No. 2, Determination of Turbidity of Water 10
4 Experiment No. 3, Determination of Dissolved Oxygen (DO) in Water 14
5 Experiment No. 4, Determination of Total Solids in Water 17
Experiment No. 5, Determination of Amount of Sodium & Potassium in

6 21
Water using Flame Photometer
7 Experiment No. 6, Determination of Hardness of a Water Sample 24
8 Experiment No. 7, Determination of Chlorides in a Water Sample 29
9 Experiment No. 8, To determine the BOD. 34
10 Experiment No. 9, To determine the COD of water sample. 38
Experiment No. 10, To determine the amount of Nitrogen by Kjedhal

11 43
method.
Experiment No. 11, To determine the amount of Sulphates by
12 48
Turbidimetric method
13 Experiment No. 12, To determine the alkalinity of water. 51
Experiment No. 13, To determine the amount of chlorides in water by

14 59
mercuric nitrate method.
Page | 3
List of Equipment
Sr. No. Description
1 Kjeldhall Nitrogen Apparatus
2 Flame Photometer
3 Incubator-1
4 Incubator -2
5 Autoclave
6 Refrigerator
7 Microwave Oven
8 Water Bath
9 Desiccator
10 Filtration Assembly
11 Measuring Balance
12 Turbidity Meter
13 DO-Meter
14 TDS-Meter
15 PH & EC Meter
Page | 4
16 Burette
17 Air Pump
18 Imhoff Cone
19 Water Distillation Assembly
20 Microscope
21 Muffle Furnace
22 Hot Plate With Magnetic Stirrer
Page | 5
EXPERIMENT # 01
Determination of pH of water sample
Purpose
 To determine pH value of the water sample in the laboratory
Standard Method No
 4500-H+ B
Reference
 A.D. Eaton, L.S. Clesceri, E.W. Rice, A.E. Greenberg, Standard methods for the examination of
water & waste water, 21 ed., (2005).
Apparatus
 Product Name: Digital Multi-parameter meter
 Model: inoLab Multi 9420
 Manufacturer: WTW (Germany)
 Functions: It measures
 pH
 Electrical Conductivity (µS/cm)
 Temperature (oC)
Related Theory
pH
pH of pure water
Page | 6
pH adjustment
Representative pH values
Substance pH
Hydrochloric acid, 10M -1.0
Lead-acid battery 0.5
Gastric acid 1.5 – 2.0
pH Measurement Lemon juice 2.4
Cola 2.5
Vinegar 2.9
Orange or apple juice 3.5
Tomato Juice 4.0
pH and Temperature Beer 4.5
Acid Rain <5.0
Coffee 5.0
Tea or healthy skin 5.5
Standard Guidelines Urine 6.0
Milk 6.5
Pure Water 7.0
Healthy human saliva 6.5 – 7.4
Blood 7.34 – 7.45
Seawater 7.7 – 8.3
Procedure inclusive of Calibration Hand soap 9.0 – 10.0
Bleach 12.5
1. Switch on the instrument.
2. Calibrate the instrument with standard solutions while the display is on.
3. For this purpose, Buffer Solutions (pH 4, pH 7, pH 10) are used as standard solution for calibration, if
required.
4. After the calibration, take that sample whose pH or EC is to be determined.
5. Insert specific glass electrode probe (either pH or EC) in the solution and wait for 5-10 minutes while
blinking the screen stop and stabilize. Note the reading.
6. Take the glass probe out from the solution and place again in standard buffer solution.
7. Take the glass probe out from the solution and rinse it gently with distilled water and place again in
buffer solution (KCl).
Observations and Calculation
Sample No. Sample Type pH
Page | 7
Comments
Questions
1. What are the applications of pH test in environmental engineering?
2. Express the following pH into hydrogen ion concentration

pH 2, pH 10 and pH 4.5
3. What is the guideline value of pH for drinking water?
4. Why pH changes in the presence of algal blooms?
5. Define pH?
Page | 8
EXPERIMENT # 02
Determination of Turbidity of Water
Purpose
 To determine the turbidity of the water sample in the laboratory
Standard Method No
 2130 B
Reference
Apparatus
 Product Name: Portable Turbidimeter

 Model: Turb 430 IR/T
 Manufacturer: WTW (Germany)
 Principle: Nephelometry:
Measure light deflected at an angle of 90o from the
sample & light source.
Related Theory
Turbidity
Causes of Turbidity
Why do we measure Turbidity?
Page | 9
Standard Guidelines
Procedure inclusive of Calibration
 Switch on the instrument
 When display is on then calibrate the instrument with following standard solutions, if
required:
1. 1000 NTU
2. 10 NTU
3. 0.02 NTU
 After the calibration, clean the glass cell (rinse with distilled water).
 Wash the cell with sample to be measured.
 Fill the cell with 15 ml of sample.
 Rotate and align the cell into its designated position with 60° angle variance and wait
until the reading is constant.
 Note down the reading.

 Remove the cell outside and rinse it with distilled water
Observations and Calculations
Sr Turbidity (NTU)
Sample Name Angle
# Reading 1 Reading 2 Reading 3
1 0
60
120
180
240
300
360
Final Value of Turbidity = NTU
2 0
Page | 10
60
120
180
240
300
360
3 0
60
120
180
240
300
360
4 Filtered Water 0
60
120
180
240
300
360
Comments
Questions
Page | 11
1. Compare Jackson candle and Nephelometric method?
2. What are the major contributors towards the turbidity of water?
3. What would be the effect of turbid water on the disinfectant ability?
4. What are the Colloidal particles?
Page | 12
EXPERIMENT # 03
Determination of Dissolved Oxygen (DO) in Water
Purpose
 To determine the DO level of the water samples in the laboratory
Standard Method No
 2430 B
Reference
water & waste water, 21 ed., (2005)
Apparatus
 Product Name: DO Meter

 Model: DO 200A
 Manufacturer: Eco Sense (USA)
 DO (ppm)
 Percentage Saturation (%)
% age Saturation = (DO/Saturation Level) x 100
Working:
Recall Mode Del
To save any measurement, press the button.
To check your saved value, go to Mode Recall
Press button.
To delete away any stored value, go to Mode
Del Press button.
Range of DO meter:
 0  20 ppm for DO
 -6  46 oC for Temperature
 0  200 % for percentage saturation.
Related Theory
Page | 13
DO
Significance
Factors affecting DO
Standard Guidelines
Procedure inclusive of Calibration
 Switch on the instrument.

 Remove the protective cap of DO probe and rinse it with distilled water.
 Press CAL Button by increasing or decreasing pressure to calibrate it, till creates 100% water-
saturated air environment i.e., 1013 atm.
 After the calibration, take that sample whose DO is to be determined.
 Insert electrode probe in the solution and wait for 5-10 minutes when blinking on the screen stop and
stabilize.
 Take the glass probe out from the solution, rinse it with distilled water and cover the probe with
protective cap again.
Page | 14
Sr # Sample Location DO (ppm) Temperature °C % Saturation
Page | 15
Comments
Questions
1. What are the factors upon which solubility of oxygen depends?
2. Write the significance of this test in Environmental Engineering?
3. What is optimum DO value set in the secondary biological wastewater treatment plant?
Page | 16
EXPERIMENT # 04
Determination of Total Solids in Water
Purpose
 To determine the total solids in water samples in the laboratory.
Standard Method No
 2540 C
Reference
Apparatus for TDS

 Product Name: Handheld TDS/Temperature meter
 Model: CON 5/TDS
 Manufacturer: Eutech (Singapore)
 TDS (ppm)
Apparatus for TSS:
 Filter paper
 0.2um for water
 0.45um for Waste water
 Dessicator
 Drying Oven
 Weighing balance (220g and 2000g)
 Filtration Assembly
 Petri Dish
 Vacuum Pump
Related Theory
TS-Total Solids
Comparison between TSS And TDS:
Page | 17
Procedure for TDS inclusive of Calibration
 Switch on the instrument

 When display is on then calibrate the instrument.
 Calibration procedure: Press the hold/enter button for the TDS Conversion Factor, for our case 67
according to Manual. (50 – 80 range)
 After setting the conversion factor dip the electrode in a standard buffer solution of 442
ppm.
 The calibration will be completed after viewing the “Calibration Successful” on the
display screen.
 After calibration, take the sample who’s TDS is to be determined.
 Insert electrode probe in the solution and wait for 5-10 minutes when blinking is stop and stabilize.
 Take the glass probe out from the solution, rinse with distilled water and place it back in the box.
Procedure for TSS
1. Weighting the filter paper using electronic balance.

2. Take the sample of distilled water.
3. Place the filter paper in the filtration assembly.
4. Pour the given sample of water into the assembly.
5. Turn on the vacuum pump to remove any air/vacuum and to allow proper filtration.
6. After the filtration remove the filter paper.
7. Place the filter paper in drying oven at a temperature of 103 oC to 105 oC for one hour.
8. Remove the filter paper from the oven and place it in a desiccator for 20 minutes to balance the
temperature and pressure.
9. Weight the filter paper and designate the weight in grams as B.
10. Repeat the same procedure for the desired sample (canal water). Designate the weight as A.
( )
TDS Calculations
Sample TDS Reading (mg/L)
TSS Calculations
Weight of filter paper =

Weight of filter paper + Residue =
Volume of sample =
Page | 18
TSS = (A - B) x 1000 / Volume of sample

TSS = ppm (mg/L)
Comments
Questions
1. Why sample is evaporated at 180 oC for dissolved solids?
2. What is the WHO guideline value for total solids?
3. Define volatile solids?
4. What is a gravimetric method?
5. Why some solids settle down after some time?
Page | 19
EXPERIMENT # 05
Determination of Amount of Sodium & Potassium in Water using Flame Photometer
Purpose
 To determine the amount of Sodium & Potassium in the water samples in the laboratory.
Standard Method No
 3500-Na D for Sodium and 3500-K B for Potassium
Reference
Apparatus
 Product Name: Flame Photometer

 Model: M360
 Manufacturer: Sherwood Flame Photometer
 Applications: Can be used to determine the amount of Na, K, Li, Ba (in
ppm)
 Other Apparatus:
 Gas cylinder
 Beaker
 Vacuum Pump
Related Theory
Working Principle of Flame photometer
General application of Flame photometer
Components of Flame photometer
Page | 20
Reagents
Standard Guideline
Procedure
1. Turn on the air supply as well as the gas supply from the cylinder.
2. Place a beaker of distilled water on the right side of the flame photometer and insert the nebulizer
in the beaker.
3. The meter will display a certain reading.
4. With the help of the blank control set the value to zero.
5. Now replace the distilled water with the standard stock solution and with the help of fine control
adjust the value as per the concentration of the standard solution.
6. Again place the distilled water. If the meter shows zero reading, it means that the calibration is
OK, otherwise again prepare the standard stock solution.
7. After the calibration is done place the desired sample and record the readings in ppm.
Sample Sodium Potassium
Comments
Questions
1. What is Pseudo hardness?
2. What would be the effect of higher concentration of sodium & potassium in water?
Page | 21
3. What are the advantages of sodium & Potassium in water?
4. WHO guidelines for the sodium & Potassium in drinking water?
5. What is the concentration of Sodium & Potassium in fresh water and distilled
water?
Page | 22
EXPERIMENT # 06
Determination of Hardness of a Water Sample
Purpose
 To determine the total Hardness, Calcium Hardness, Magnesium Hardness of different water
samples by EDTA (Ethylene Di-amine Tetra Acetic Acid) Method.
Standard Method No
 2340 C
Reference
 A.D. Eaton, L.S. Clesceri, E.W. Rice, A.E. Greenberg, Standard methods for the
examination of water & waste water, 21 ed., (2005).
Apparatus
 Titration flask
 Burette and Pippete
 Different buffer solutions and indicators
Related Theory
Hard Water
Page | 23
Titration Theory
Standard Guidelines
Procedure
Hardness can be determined by Complexo-metric titration.
Total Hardness
1. Take 25 ml of water sample in Titration Flask.

2. Add 25 ml Distilled water in it to dilute the water solution (to avoid formation of CaCO 3). Distilled
water does not participate in ion exchange in reaction.
3. Add 1 - 2 ml of Buffer Solution (Ammonia Buffer NH4Cl + NH4OH) to maintain pH in solution 7 - 9.
4. Add small amount of EBT (Ecrichrome Black T) as indicator. As a result of addition of EBT, solution
of color changes to wine red.
5. Titrate it against 0.01M EDTA solution. Add EDTA (Ethyle Diamine Tetra Acetic Acid) from burette
until color changes to blue.
6. Test three samples and determine mean volume of titrant used.
7. Total Hardness (mg/lit) as CaCO3 is calculated from the following formula.
mean vol of titrant used x molarity of EDTA x MW of CaCO3 x 100

Total Hardness in mg/l as CaCO3 
vol of sample in ml
Molarity of EDTA =
Volume of sample used =
MW of CaCO3 =
Calcium Hardness
1. Take 25 ml of water sample in Titration Flask.

2. Add 25 ml Distilled water in it to dilute the water sample.
Page | 24
3. Add 2 - 3 ml of NaOH Buffer Solution.

4. Add small amount of EBBR (Ecrichrome Blue Black R) as indicator. As a result of addition of
EBBR, colour of solution changes to wine red.
5. Titrate it against 0.01M EDTA solution. Add EDTA (Ethylene Di-amine Tetra Acetic Acid) from
burette until colour changes to blue.
6. Test three samples and determine mean volume of Titrant used.
7. Calcium Hardness (mg/lit) as CaCO3 is calculated from the following formula:
mean vol of titrant used x molarity of EDTA x MW of CaCO3 x 1000

Calcium Hardness in mg/l as CaCO3 
vol of sample in ml
Molarity of EDTA =
MW of CaCO3 =
Magnesium Hardness
Total Hardness = Calcium Hardness + Magnesium Hardness
Magnesium Hardness = Total Hardness - Calcium Hardness
Calcium Ions
Procedure is same as above for Calcium Hardness
Calcium Ions (mg/lit) is calculated from the following formula:
mean vol of titrant used x molarity of EDTA x MW of Ca x 1000
Calcium Ions in mg/l 
vol of sample in ml
Molarity of EDTA =
MW of Ca =
Observations & Calculations
Total Hardness as CaCO3 (mg/l) = (Vol. of Titrant used x 1000) / Vol. of sample
Calcium Hardness as CaCO3 (mg/l) = (Volume of Titrant used x 1000)/Volume of sample
Magnesium Hardness as CaCO3 (mg/l) = Total Hardness as CaCO3 - Ca Hardness as

CaCO3
Calcium Ions (mg/l) = (Volume of Titrant used x 400.8) / Volume of sample
Total Hardness = Ca Hardness + Mg Hardness
Mean
Volume of Volume of Total Hardness
Sample Sample Volume of
Titrant used sample used as CaCO3
No. Description Titrant used
(ml) (ml) (mg/l)
(ml)
Page | 25
Lab prepared
1 Sample 1
Lab prepared
2 Sample 2
Filter water
3
Volume Calcium
Volume Magnesium
of Mean Hardnes Calcium
Sample Sample of Hardness
Titrant Volume s as ions
No. Description sample as CaCO3
used (ml) CaCO3 (mg/l)
(ml) (mg/l)
(ml) (mg/l)
Lab
1 prepared
Sample 1
Lab
2 prepared
Sample 2
3 Filter water
Comments
Questions
1. What is pseudo hardness?
2. Why hardness is always calculated in terms of CaCO3?
3. What causes hardness in water?
4. Why NaOH is used in the determination of Calcium hardness?

5. The EDTA titration is known as complexometric titration” Why?
6). How temporary & permanent hardness is removed from the water sample
Page | 26
EXPERIMENT # 07
Determination of Chlorides in a Water Sample
Purpose
 To determine the chloride concentration in different water samples
Standard Method No.:
 4500-Cl C
Reference
Apparatus
 Titration flask
 Burette and Pippete
 Different buffer solutions and indicators
Related Theory
Chlorides
Chlorides in Water
Methods of determination of Chlorides
Page | 27
Mercuric Nitrate Method

Principle
Interference
Standard Guideline
Procedure
a. Titration of chloride concentrations less than 100 mg/lit:
1. Take a 100-ml of chloride containing solution in titration flask (100ml chloride containing sample
is taken because of this sample contains less amount of chlorides)
2. Add 1.0 ml indicator-acidifier reagent. It is a mixture of diphenyl carbazone and Xylene cyanol.
If
pH < 2.30 then the color of the solution will be green

pH = 2.30 to 3.80 then the color of the solution will be bluish green
pH > 3.80 then the color of the solution will be blue
3. Titrate this sample with 0.0141N Hg(N03)2 titrant till a definite purple end point color achieved.
4. We can use high strength 0.141N Hg(N03)2 instead of 0.0141N Hg(N03)2 as a titrant but after few
drops the definite purple end point color will be achieved. So it requires care.
5. Take three readings and determine mean volume as A.
6. Take 100-ml distilled water in titration flask.
7. Add indicator (diphenyl carbazone + Xylene cyanol) + 10mg Na2C03.
8. Titrate this sample with 0.0141N Hg(N03)2 titrant till a definite purple end point color achieved.
9. Take only reading and determine volume of the titrant Hg(N03)2 used as B.
10. Chloride ions concentration can be determined from following formula
(A  B) x N x EqW of Cl - x 10000
Cl - in mg/l 
vol of sample in ml
where:
A = mean volume of Hg(N03)2 in ml used to titrate the sample
B = mean volume of Hg(N03)2 in ml used to titrate the distilled water
N = normality of Hg(N03)2 i.e 0.0141N Hg(N03)2
b. Titration of chloride concentrations greater than 100 mg/lit:
1. Take a 50-ml of chloride containing solution in titration flask.

2. Add 0.5 ml mixed indicator. It is a mixture of di-phenylcarbazone and bromophenol.
3. Add few drops of 0.1N HN03 till color become yellow.
Page | 28
4. Titrate this sample with high strength 0.141N Hg(N03)2 titrant till a definite purple end point
color achieved.
5. Take three readings and determine mean volume as A.
6. Take 50-ml distilled water in titration flask.
7. Add indicator
8. Titrate this sample with 0.0141N Hg (N03)2 titrant till a definite purple end point color achieved.
9. Take only reading and determine volume of the titrant Hg(N03)2 used as B.
10. Chloride ions concentration can be determined from following formula
(A  B) x N x MW of Cl - x 10000
Cl - in mg/l 
vol of sample in ml
where:
A = mean volume of Hg(N03)2 in ml used to titrate the sample
B = mean volume of Hg(N03)2 in ml used to titrate the distilled water
N = normality of Hg(N03)2 i.e 0.10N Hg(N03)2
Observations & Calculations
For Cl- concentration > 100 mg/lit
Initial Final Volume

Mean Volume Cl-
Sample Reading Reading of Titrant
Volume of sample Concentration
No. from from used
(ml) (ml) (mg/l)
Burette Burette (ml)
Comments
Page | 29
Questions
1. What is the WHO guideline value for chlorides?

2. What is the significance of chlorides test for construction purposes?
.
3. How chlorides gain access to natural waters?

4. What would be the role of mixed indicator in this titration?
5. Why different procedures are used depending upon chlorides concentration?
Page | 30
EXPERIMENT NO. #08

TO DETERMINE THE ALKALINITY OF WASTEWATER
STANDARD METHOD NO
 2320 B
REFERENCE
RELATED THEORY
ALKALINITY
BUFFER SOLUTIONS
REASONS FOR ALKALINITY
MAJOR CONTRIBUTOR TOWARDS ALKALINITY
Page | 31
METHOD OF DETERMINING ALKALINITY
METHODOLOGY
INTERFERENCES
REAGENTS:
PROCEDURE
(A) PHENOLPHTHALEIN ALKALINITY
1. Take 50 m1 sample.
2. Add 2-3 drops of phenolphthalein in a titration flask if pink colour present.
3. Titrate over a white surface with 0.02 N H2SO4 to a colourless endpoint.
(B) METHYL ORANGE ALKALINITY
1. In the same flask add 2-3 drops of methyl orange indicator.

2. Titrate with 0.02 N H2SO4 until the colour changes to orange.
3. Take at least three readings for A and B and calculate the alkalinity by the formula given below:
Alkalinity (mg/l) = (A x N x 50000) / (ml of sample)
Where,
A = Volume of Titrant used
N = Normality of Acid (0.02) or N/50 H2SO4
mL of sample used = ml
Page | 32
ALKALINITY READINGS
Volume of Mean Volume of

Sample Sample Alkalinity of
Titrant used Volume sample
no Name sample
(ml) (ml) (ml)
Lab prepared
1
1
Lab prepared
2
2
3 Tap water
COMMENTS
Questions:
1. Why alkalinity is measured as CaCO3 Eq?
2. Write applications of alkalinity measurement?
3. Why alkalinity is known as buffering capacity of water?
4. What is the importance of alkalinity in chemical coagulation?
5. Write down application of alkalinity data in water softening?
Page | 33
Experiment No. # 09
TO DETERMINE THE BOD IN A DOMESTIC WASTE WATER SAMPLE
STANDARD METHOD NO
 5210 B
REFERENCE
RELATED THEORY
BIOCHEMICAL OXYGEN DEMAND (BOD):
BOD Level (in ppm) Water Quality
IMPORTANCE OF BOD TEST IN ENVIRONMENTAL ENGINEERING:
Page | 34
DETERMINATION OF BOD
PRINCIPLE
SAMPLING AND STORAGE
APPARATUS
 Incubation bottles: Use glass bottles having 60 ml or greater capacity (300 ml bottles having ground-
glass stopper and a flared mouth are preferred).
 Air incubator or water bath, thermo-statistically controlled at 20 ± 1°C. Exclude all light to prevent
possibility of photosynthetic production of DO.
REAGENTS
Page | 35
PROCEDURE: (WITHOUT SEEDING)
1. First of all it is important to know the amount of samples to be used for test. For this purpose the
source of sample is to be recorded which will indicate the approximate value of BOD 5 for the
sample.
(i) Domestic sewage BOD5 =100-500mg/L
(ii) Effluent from treatment plant= 20-80mg/L
(iii) River water = 2-4mg/L
2. Take 9 BOD bottles note their numbers and arrange them in 3 groups.
3. Fill each bottle half with dilution media ensuring that no air gets mixed with the media while fill
in as in DO test.
4. Add 2ml sample in each of the three bottles marked as first group; 5 ml in each bottle of 2nd group
and 10ml in each bottle of the 3rd group.
5. Fill the bottle completely with dilution media and place the stopper such that no air bubbles are
trapped.
6. Now take one bottle from each set and estimate its DO. This will be DO initial or DO 0 (zero)
day.
7. For comparison prepare two more bottles with blank dilutions media (with out sewage sample)
and find the DO from one bottle.
8. Place the rest of the six bottles with sewage samples and one bottle for blank in the incubator at
200C.
9. After 5 days find out DO in all bottles.
10. That value of oxygen depletion should be considered correct which gives an oxygen depletion of
at least 2 mg/L after 5 days of incubation.
11. Calculate BOD5 at 200C. for the sample using following relationship.
BOD(mg/L) = DO depletion (mg/L) x 300

Volume of sample in bottle (ml)
OBSERVATIONS & CALCULATIONS
At zero day
Volume of
Sample Total Volume DO
Bottle # Titrant used
added (ml) of Media (ml) (mg/L)
(mL)
1
2
3
B1
Page | 36
After 5 days
Volume of
Sample Volume of DO Mean DO
Bottle # Titrant used
added (ml) sample (ml) (mg/L) (mg/L)
(mL)
4
5
6
7
8
9
B2
DO Depletion
DO at Zero DO at 5 DO
Sample BOD5
days days Depleted
added (ml) (mg/L)
(mg/L) (mg/L) (mg/L)
2
5
10
Average Reading of BOD =
Comments
Page | 37
Questions:
1). Define BOD?
2) What is the permissible value of NEQs for BOD of discharge waters into the streams?
3) What is the role of nitrifying bacteria in BOD test?
4) Why aeration is important for dilution media?
5) Give any three differences between COD & BOD?
BOD COD
Page | 38
Experiment No. # 10
TO DETERMINE THE AMOUNT OF CHEMICAL OXYGEN DEMAND (COD) IN A WASTEWATER

SAMPLE
STANDARD METHOD NO
 5220 A
REFERENCE
RELATED THEORY
CHEMICAL OXYGEN DEMAND (COD)
METHODS OF DETERMINATION OF COD
OPEN REFLUX TITRIMETRIC METHOD
PRINCIPLE
EQUIPMENT
CAUTION: The presence of minute traces of organic matter on the equipment will cause large errors in the
test results. So clean all equipment thoroughly before using.
 Erlenmeyer flask
 Small beaker
 Titration apparatus:
 25 or 50 mL burette, graduated in 0.1 mL
 burette support
Page | 39
 100 mL graduated cylinder

 rubber-tipped stirring rod, or magnetic stirrer and stir bar
 white porcelain evaporating dish, 4.5 inches in diameter
 Reflux apparatus:
 500 or 250 mL Erlenmeyer flasks with ground glass 24/40 neck

 300 mm jacket Liebig, West, or equivalent condenser with 24/40 ground-glass
joint
 hot plate with sufficient power to produce at least 1.4 W /cm2 of heating surface
 Blender
 Pipets
 Glass beads
 Microwave oven
REAGENTS
THEORY OF TITRATION
Page | 40
INTERFERENCES
PROCEDURE
1. Place 50ml sample in 500ml refluxing flask (for samples with COD > 900mg/L use a smaller
sample diluted to 50 ml).
2. Add 1g HgSO4 and several glass beeds.
3. Add slowly 5ml H2SO4 reagent while mixing to dissolve HgSO4
4. Cool while mixing to avoid the loss of volatile materials.
5. Add 25 ml 0.25N K2 Cr2O7 solution and mix.
6. Attach the flask to the condenser and turn on cooling water.
7. Add remaining H2SO4 (70ml) through open end of the condenser continue mixing while adding
H2SO4 reagent.
8. Place the mixture for 2 hrs in oven and cool to room temperature. Then dilute the mixture to
about 200 mL with distilled water.
9. Titrate excess of K2Cr2O7 with Ferrous ammonium sulfate using 2,3 drops of ferrion indicator.
The end point will be from blue green to reddish brown.
10. Reflux and titrate in the same manner a blank containing the reagents and the voume of the
distilled water will be equal to that of sample.
OBSERVATIONS AND CALCULATIONS:
COD (mg/L) = (A - B) x N x 8,000 / (Volume of Sample, ml)
Where,
A = ml of titrant used for Blank
B = ml of titrant used for Sample
N = normality of ferrous ammonium sulfate (FAS) = 0.25N
8000 = Equivalent wt. of Oxygen x 1000
Volume of Volume of
Description of
Sr. No. titrant used for titrant used for COD
Sample
sample blank
ml ml mg/litre
Page | 41
Comments
Questions
1) Why COD values are always higher then BOD values?
2) Write the applications of COD data to Environmental Engineering?
3) Write the NEQS for COD in discharge wastewater to stream?
4) What would be the role of Ag2SO4 in COD determination?
.
5) What would be the COD values for industrial textile wastewaters? Compare them
with COD values of domestic wastewater?
Page | 42
Experiment No. # 11
TO DETERMINE THE AMOUNT OF KJELDHAL NITROGEN IN A GIVE WASTEWATER SAMPLE
STANDARD METHOD NO
 4500-Norg
REFERENCE
RELATED THEORY
GENERAL
PRINCIPLE
TITRATION THEORY
REAGENTS
Page | 43
PROCEDURE
1. DIGESTION
1. Take 280ml of sample in a kjeldhal flask.

2. Add few glass beads to it then add 50ml digestion reagent
3. Mix, heat and continue boiling until solution remains 25-50ml.
4. Cool it and add 280 mL distilled water to it to make the volume approx. 300ml.
5. Add 0.5 ml phenolphthalein indicator.
6. Add 50 ml thiosulfate hydroxide reagent solution.
7. If pink colour does not appears then add more 50ml thiosulfate hydroxide reagent solution.
2. DISTILLATION
1. In collect the distillate in a flask containing boric acid solution.
2. Collect 200ml distillate into 50ml boric acid solution.
3. TITRATION
1. Titrate it against 0.02N H2SO4 solution until colour changes from purple to green.
2. Carry the blank titration, following all steps of procedure.
Calculations
Total Nitrogen (mg/L) = (A - B) x 280

ml of sample
A = Volume of H2SO4 used for sample = ml
B = Volume of H2SO4 used for blank = ml
Total nitrogen (mg/L) = mg/lit
Comments
Page | 44
Questions
1. What is Kjeldhal nitrogen?
2. What is blue baby disease?
3. How ammonia nitrogen can be determined?
4. Why hydroxide thiosulfate reagent is added in above experiment?
5. Write the NEQS for TKN in discharge wastewater to stream?
Page | 45
EXPERIMENT # 12
TO DETERMINE TOTAL COLIFORM AND FECAL COLIFORM BY MULTIPLE TUBE FERMENTATION
TECHNIQUE
STANDARD METHOD NO
 9221 C
REFERENCE
RELATED THEORY
TOTAL COLIFORMS
PURPOSE
LIMITATIONS
Page | 46
STANDARD PRESUMPTIVE METHOD
APPARATUS
 Autoclave
 Incubator
 Sample bottles
 Fermentation tubes with inverted vials
 Dilution bottles
 Pipettes and pipette stand
REAGENTS
PROCEDURE
 For potable water arrange ten fermentation tubes in rack with inverted vials. Before sterilization,
dispense sufficient medium, to cover inverted vials at least partially after sterilization;
 Sterilize the fermentation tubes containing the medium along with other necessary glass apparatus
in an autoclave for 15 minutes at 1210C;
 Remove fermentation tubes from autoclave as soon as the chamber pressure reaches to zero.
Never re-autoclave the medium;
 Dispense 10 ml of sample in each tube and incubate inoculated tubes at 35  0.50C. After 24  2
hours shake each tube gently and examine it for gas or acidic growth. If no gas or acidic growth
has formed, re-incubate and re-examine at the end of 48  2 hrs. Record the presence or absence
of gas or acid production in the fermentation tubes;
 Absence of acidic growth or gas formation at the end of 48  2 hours of incubation constitute a
negative test;
 Production of gas or acidic growth in the tubes within 48  2 hours constitutes a positive
presumptive reaction. Submit these tubes with a positive presumptive reaction to the confirmed
phase;
Page | 47
 Shake sample and dilutions vigorously about 25 times and repeat same procedure mention as for
portable or drinking water.
CONFIRMED PHASE
REAGENT
APPARATUS
 Fermentation tubes with caps
 Inverted vials
 Sterile metal loop 3 mm in diameter
 Sprit Lamp
PROCEDURE
 Before sterilization, dispense sufficient medium, to cover inverted vials at least partially after
sterilization.
 Submit all primary tubes showing any amount of gas or acidic growth with in 242 or 48 2
hours of incubation to the confirmed phase.
 If active fermentation or acidic growth appears in the primary tubes earlier than 24 hours, transfer
to the confirmatory medium, preferably without waiting for the full 24 2 hours period to elapse.
 If additional primary tubes show acidic growth at the end of a 48 2 hours incubation period,
submit these to the confirmed phase;
 Gently shake or rotate primary tubes showing gas or acidic growth to re-suspend the organisms.
 Take a metal inoculating loop of 3 mm diameter and heat it on the sprit lamp till it becomes red-
hot;
 Cool the loop to room temperature and with its help transfer one loop full of culture to a
fermentation tube containing brilliant green lactose bile broth.
 Incubate the inoculated Brilliant Green Lactose Bile Broth tube for 48  2 hours at 35  0.50C.
 Formation of gas in any amount in the inverted vial of the brilliant green lactose bile broth
fermentation tube at any time with in 48  2 hours constitute a positive confirmed phase.
 Calculate the MPN value from the number of positive brilliant green lactose bile tubes as
Page | 48
FECAL COLIFORM
DEFINITION
PURPOSE
LIMITATIONS
REAGENTS
APPARATUS
 Fermentation tubes with caps
 Inverted vials
 Sterile metal loop 3 mm diameter
 Sprit Lamp
PROCEDURE
Page | 49
 Before sterilization dispense in fermentation tubes each with an inverted vial sufficient medium
to cover the inverted vial at least partially after sterilization. Close tubes with caps.
 Sterilize the tubes containing medium and other necessary glassware at 1210C for 15 minutes in
an autoclave.
 Submit all presumptive fermentation tubes showing any amount of gas or heavy growth with in
48 hours of incubation to the confirmed test.
 Gently shake or rotate presumptive fermentation tubes showing gas or heavy growth;
 Take a 3 mm diameter metal loop and heat to red-hot on the sprit lamp.
 Cool the loop to room temperature and with the help of this loop transfer growth from each
presumptive fermentation tube to EC broth.
 Incubate inoculated EC broth tubes at 44.5  0.20C for 24  2 hours.
 Gas production in an EC broth culture with in 24 hours or less is considered a positive fecal
Coliform reaction.
 Failure to produce gas (growth sometimes occurs) constitute a negative reaction indicating a
source other than the intestinal trace of a warm-blooded animals.
OBSERVATIONS AND CALCULATIONS:
Lactose Brothe (PresumtiveTest)
Volume of Lactose
Sr Total Positive Negative
Sample Brothe
No. Tubes Tubes Tubes
Used Solution
1
2
3
BGBB (Total Coliform)
Volume of
Sr Total BGBB Positive Negative
Sample
No. Tubes Solution Tubes Tubes
Used
Page | 50
1
2
3
Total Coliform (MPN / 100 ml) = MPN
E.C. Brothe (Fecal Coliform)
Volume of
Sr Total BGBB Positive Negative
Sample
No. Tubes Solution Tubes Tubes
Used
1
2
3
Fecal Coliform (MPN / 100 ml) = MPN
Comments:
Questions:
1. What are bacteria?
2. What are the WHO guidelines for microbiological quality of drinking water?
Guideline
Organism Unit Remarks
value
E-Coli
Coliform
Coliform
Page | 51
3. Compare bacteria with aquatic plants?
Sr. # Bacteria Aquatic Plants

1
4. Name some diseases caused by bacteria?
5. What are indicator organisms?
Page | 52
Experiment No. # 13
TO DETERMINE THE AMOUNT OF SULFATES IN A GIVEN WATER SAMPLE
STANDARD METHOD NO
 4500-SO42- E
REFERENCE
RELATED THEORY
.
METHODS OF ANALYSIS
.
TURBIDIMETRIC METHOD
APPARATUS
PROCEDURE
1. Formation of magnesium sulfate turbidity:
Page | 53
2. Measurement of magnesium sulfate turbidity:
3. Preparation of calibration curve:
4. Correction for sample color and turbidity:
OBSERVATIONS & CALCULATIONS
Sulfates (mg/L) = mg SO4-2 x 1000

ml of sample
Dilution factor = ml of sample + ml of water added

ml of sample
Sample type = Wastewater
Concentration of
Sr. No. Turbidity (NTU)
Sulfate (mg/L)
1
2
3
4
5
6
Sample A=?
Page | 54
20
18
16
y = 0.0247x + 1.5711
14
Turbidity (NTU)
R² = 0.9954
12
10
8
6
4
2
0
0 100 200 Sulfate
300 Concentration
400 500
(mg/L) 600 700 800
Concentration of sulfates from the equation of calibration curve A (mg/L) = mg/L
Comments
Questions:
1. Write the public health significance of sulfates.
2. What should be the material of structure to be used to hold sulphate containing

waste water?
.
3. Discuss the odor problem associated with sulfates presence in water?

.
4. What are the basic causes of sulfate in water?
5. Discuss the corrosion of sewers?
Page | 55

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ENVIRONMENTAL ENGINEERING

DEPARTMENT OF CIVIL ENGINEERING,

Created by: Engr. Ali Zulqarnain

Last Updated by: Engr. Rizwan Amjad

Approved by the HoD: Dr. Shahid Ali

Sr. No. Description Page No.

2 Experiment No. 1, Determination of pH of water sample 6

3 Experiment No. 2, Determination of Turbidity of Water 10

4 Experiment No. 3, Determination of Dissolved Oxygen (DO) in Water 14

5 Experiment No. 4, Determination of Total Solids in Water 17

Experiment No. 5, Determination of Amount of Sodium & Potassium in

7 Experiment No. 6, Determination of Hardness of a Water Sample 24

8 Experiment No. 7, Determination of Chlorides in a Water Sample 29

9 Experiment No. 8, To determine the BOD. 34

10 Experiment No. 9, To determine the COD of water sample. 38

Experiment No. 10, To determine the amount of Nitrogen by Kjedhal

13 Experiment No. 12, To determine the alkalinity of water. 51

Experiment No. 13, To determine the amount of chlorides in water by

Sr. No. Description

1 Kjeldhall Nitrogen Apparatus

19 Water Distillation Assembly

22 Hot Plate With Magnetic Stirrer

Sample No. Sample Type pH

2. Express the following pH into hydrogen ion concentration

3. What is the guideline value of pH for drinking water?

4. Why pH changes in the presence of algal blooms?

 To determine the turbidity of the water sample in the laboratory

 Product Name: Portable Turbidimeter

Why do we measure Turbidity?

Procedure inclusive of Calibration

 Switch on the instrument

 Wash the cell with sample to be measured.

 Fill the cell with 15 ml of sample.

 Note down the reading.

Observations and Calculations

1. Compare Jackson candle and Nephelometric method?

2. What are the major contributors towards the turbidity of water?

3. What would be the effect of turbid water on the disinfectant ability?

4. What are the Colloidal particles?

 To determine the DO level of the water samples in the laboratory

 Product Name: DO Meter

Procedure inclusive of Calibration

 Switch on the instrument.

Observations and Calculations

Sr # Sample Location DO (ppm) Temperature °C % Saturation

2. Write the significance of this test in Environmental Engineering?

Apparatus for TDS

Comparison between TSS And TDS:

Procedure for TDS inclusive of Calibration

 Switch on the instrument

1. Weighting the filter paper using electronic balance.

Observations and Calculations

Sample TDS Reading (mg/L)

Weight of filter paper =

TSS = (A - B) x 1000 / Volume of sample

2. What is the WHO guideline value for total solids?

3. Define volatile solids?

4. What is a gravimetric method?

5. Why some solids settle down after some time?