CVNG 3007

ENVIRONMENTAL ENGINEERING 1

LABORATORY MANUAL
2015 2016
The Analysis of Water and Wastewater

Prepared by: Althea Richardson (CET)

Department of Civil and Environmental Engineering
The University of the West Indies- St Augustine Campus

CONTENTS
Introduction
Safety Guidelines
Lab report format
Activity 1 - Water Analysis Lab
Test 1 - Bacteriological Analysis
Test 2 - Jar Test
Test 3 - Source Determination
pH
Total/Free Chlorine Residual
Chloride
Hardness
Alkalinity
Activity 2 - Wastewater Analysis
Test 1 - Dissolved Oxygen (DO) - Titration Method
Test 2 - Biochemical Oxygen Demand (BOD)
Test 3 - Total Suspended Solids (TSS)
Test 4 - Settleable Solids (SS)
Test 5 - pH

Activity 3 - Field Trip / Visit

1. Beetham Wastewater Treatment Plant
2. Caroni Arena Water Treatment Plant

INTRODUCTION
Water, wastewater... what's the difference?
Environmental professionals toss around the terms "water" and "wastewater" every day, without a
doubt as to their meanings. Outside of the profession however, differences in the two terms might not be
so clear.
Drinking water starts out as surface water (lake/dam/reservoir/river), groundwater or sea water.
Providers like WASA draw "raw (untreated) water" from source. It is pumped to a treatment facility or
plant where it may be chemically and or physically treated and then routed through a series of settling
tanks and filters to remove micro particles. Disinfection is done to make the finished water potable. A
large network of pumps, storage tanks and pipes is then used to transport the potable water to consumers.
Wastewater is also referred to as "sewer water". Generally, the potable water that was used to bathe,
cook, or flush becomes wastewater. A large network of collection pipes is also used to transport
wastewater from homes and businesses to treatment facilities or plants. The operations at wastewater
treatment plants are somewhat similar to what occurs at water treatment plants. The major differences are:
1.Wwastewater treatment uses biological processes to break down and remove organic matter and 2.
More settling is done to remove the natural bacteria which would have consumed the organic matter in
the wastewater. The final water is also disinfected prior to being released into a waterway.
Process Monitoring. Water and wastewater treatment requires frequent testing and monitoring of the
processes to ensure that a high quality end product is obtained and maintained. Accurate and reliable
laboratory analyses and reporting are absolutely necessary for quality control and making operational
changes.

Objectives of the Labs

These labs are designed to familiarize you, the EE student, with the common Laboratory tests and the
associated analytical skills needed to monitor environmental systems and water and wastewater treatment
processes. Some fundamental water and wastewater engineering concepts will also be illustrated.

Activities
You will be expected to complete 2 laboratory sessions and to visit 2 Treatment Plants.
ALL students must attend ALL sessions and submit reports (3) for marking. Your marks will
contribute to a percentage of your coursework marks.
Students should familiarize themselves with the laboratory schedule and other updated information
that may be posted, on the departmental notice board or myelearning, from time to time.
You are also expected to read the laboratory manual before each exercise. The more prepared you are
the more engaged and safer you will be.

GENERAL SAFETY
A lot of emphasis has been placed on making the labs as safe as possible and the lab personnel will take
the necessary precautions to prevent or reduce the occurrence of accidents. Although, safety is the
collective responsibility of all you are ultimately responsible for your own safety.
Accidents often result from an indifference to safety practices and or failure to use common sense or to
follow instructions. Each student should be aware of what others are doing because all can become
victims of one mistake. Should a laboratory accident occur, there may be significant injury to the persons
involved or anyone in the vicinity.
Do not hesitate to point out to other students that they may be engaging in an unsafe, unauthorised
practice or operation while in the lab. If necessary, report your observations to the instructor.
The most common accidents that occur in chemical laboratories are: Cuts from broken glassware or damaged equipment.
Burns from chemicals or hot surfaces.
Burns and injuries from explosions.
Skin and eye irritation caused by contact with chemicals or samples
Inhalation of toxic fumes.
Although, most of the chemicals used at this level may not be extremely hazardous there are additional
safety concerns associated with the nature and collection of the samples to be tested. Due care and
attention MUST be exercised at all times.
The safety rules given below and the additional instructions for each laboratory exercise should be
adhered to as closely as possible, at all times. Additionally, in order to ensure a successful outcome, the
laboratory personnel will give specific instructions, during each experiment, which you MUST follow

LABORATORY SAFETY RULES

Safety Equipment: On entering the laboratory please determine the location of the Eye Wash
Station, Safety Shower and Exit doors.

Hygiene: You will be exposed to sewage which could be hazardous. Handling your pens,
calculators, books, bags, phones etc. with contaminated gloves will contaminate those items. You
should make every effort to reduce your level of exposure by handling those items while working.

Use the disposable gloves provided correctly. Before use, ensure that there are no cracks or small
holes in the gloves
- If chemical diffuses through a glove and it is held against your hand you may be more exposed
than if you had not worn the glove.
- Remove gloves before leaving the lab and before handling telephones, doorknobs, writing
instruments, laptops and laboratory notebooks.

- Properly dispose of used gloves in the bins provided. Do not leave them lying around on the
desk top.

Dress appropriately for labs. Although Lab coats or aprons are not usually required, clothing worn
to labs should offer protection from splashes and spills and should be easy to remove in the event of
an accident.
- Wear old, inexpensive clothes (T shirts and jeans), safety shoes, sneakers or closed toe
shoes are an absolute MUST
- Short pants or skirts, sleeveless shirts or jerseys, tank tops, short T shirts, open toed shoes
(sandals, clogs and slippers), inappropriate fabric and jewelry will not be permitted in the
laboratory and on field trips.
- SAFETY GLASSES are allowed but not absolutely necessary.
- If you must wear contact lenses, you MUST also wear fitted goggles
- Tie long hair or braids back or up to prevent interference with your performance or that of
others.

Students WILL NOT be allowed to eat, drink, chew gum or use cell phone while in the lab.

ASK laboratory personnel for HELP to refill and to dispose of unused (waste) reagents.

Immediately report ALL spills and accidents to the laboratory personnel no matter how small or
insignificant they might appear to you.

Housekeeping: Books, bags or folders will not be allowed on the bench tops. Tidy your work area
before leaving the lab.

Before leaving the laboratory, wash hands and arms up to elbows, even if gloves were worn.

FIELD TRIP SAFETY RULES

Your field trip is an academic exercise and must be treated as such. Be prepared to treat all with
respect and to get the most out of the experience by listening and asking relevant questions.

While on the field trip adhere to ALL the safety requirements and comply with ALL instructions
given by the plant personnel.

Gear up appropriately.

Wear:a. Safety shoes, sturdy close-toed shoes or sneakers

b. Long pants or coveralls
c. Long-sleeved cotton shirt or weather-appropriate outer wear
Provide:d. Safety helmet

e. Sunscreen
f. Personal medication
g. Water and at least one healthy snack or fruit
h. Field notebook and writing implements
At all times stay within sight of the tour guide.
Do not remove anything from the site unless directed to, leave the area better than you found it.
Do not use electronic devices (cameras, cell phones, recorders) unless approval is granted.

GUIDELINES FOR THE LAB REPORTS

1. You are expected to submit three (3) reports. One for each lab (2) and one (1) for the field trip.
2. Reports should be no more than 20 typed and numbered pages (exclusive of the first page).
3. DO NOT SUBMIT YOUR CVNG 3007 REPORT IN A (MANILA OR PLASTIC) FOLDER.
Attach a cover (Title) page (see table below), staple all the pages together and submit
4. A Completed Risk Assessment Form must be included in your report.
5. REPORTS ARE DUE EXACTLY 2 WEEKS AFTER THE LAB. They should be handed to the
personnel in the Environmental Laboratory only. Five (5) marks would be deducted after the first
week outstanding and each week thereafter.

Lab Report format

A special cover page must be provided for each laboratory report. On the
cover clearly print the:

* Cover (Title) page

Abstract
Objectives
Introduction

lab title;
course name and code;
your name and ID number;
group member names;
Date performed and date submitted;
a list of items included in the report with the number of marks allocated for
each item (the cover will act as a grade sheet). [2]

A short (150 word) summary of the entire report. [2]

State the objectives of the exercise. [2]
Explain the rationale for doing the particular tests. [3]

Theory

Brief summary of the supporting theory and applications. Cite all information
used. [3]

Experimental
Procedure,
Methodology

Do not rewrite the methodology record ONLY the changes to the procedure
given in the laboratory manual that were made while doing the lab. [3]

Observations and
Results

Report your observations or findings. Where necessary, show your sample

calculations. You may use tables, graphs and drawings to present your results.
Put all test results on one summary table [10]
Photos should only be used to highlight important points and they must be
well labeled, properly cited and referenced.
Discuss the following:-

Discussion

- The environmental implications of your results;

- Your findings as compared to theory;
- The degree of confidence you can place in your results based on the
accuracy and precision you were able to obtain.
- Assumptions you might have made in your analysis and possible sources
of errors or limitations that may explain discrepancies in your results.
[10]
Avoid repeating your introduction except for purposes of reference

Conclusion

Summarize the key findings of your work and indicate whether you achieved
your stated objectives. [3]

Appendix

Use this section to put sketches of special apparatus and sample calculations and
lab data sheets [0]

Questions

Use research to provide acceptable responses to these questions which are

designed to further test your understanding of the lab. [5 x 2 = 10]

References

Cite all references used (including websites) using the proper (Chicago) style
format. [2]

NOTE:
Plagiarism is a University offense. You would be severely penalized for submitting work that
is deemed to be plagiarized from old lab reports or copied without paraphrasing and proper
citation. Be guided by the Universitys Regulations on Plagiarism

ACTIVITY 1 - Water Analysis

INTRODUCTION
The water treatment process and potable water quality is assessed, in accordance with Water Quality
Standards (WHO/EPA). The basic water treatment process can follow the flow path shown below.

SURFACE Water Treatment Plant Flow Diagram

Source: http://cof-cof.ca/wp-content/uploads/2012/03/Surface-Water-Treatment-Plant.gif

Objectives
o to demonstrate standard procedures/methods, tools, apparatus and equipment used in an
Environmental Laboratory
o to classify water based on source;
o to provide experience in analyzing laboratory test results;
o to Illustrate the shortcomings of some laboratory tests;

Learning Outcomes
At the end of this exercise the student will be able to:
Identify some of the common apparatus used in a water/wastewater lab ;
Observe laboratory safety precautions;
Perform experiments in accordance with a written laboratory procedure;
Obtain readings and measurements with minimum error;
Use water quality data to infer water quality;
Explain the water treatment process

Analysis
The following tests are to be performed on the samples provided:1. Bacteriological Analysis (using MF technique)
2. Jar test
3. Source Determination:
a. pH
b. Chlorine Residual (Total and Free)
c. Chloride
d. Hardness
e. Alkalinity

1. Bacteriological Analysis using MF Technique

Most waterborne disease-causing organisms originate in humans or animal bodies and are discharged as
part of body wastes. A primary purpose of water and wastewater treatment is to reduce or eliminate the
possible transmission of waterborne diseases by pathogens.
Although, it is very difficult to isolate and identify the disease-causing bacteria in a water laboratory, it is
possible to isolate and monitor the coliforms which are indicator organisms.
What is an indicator organism?
The MF test is used by public health and other regulatory agencies to assess the bacteriological quality of
water supplies and to establish whether there is conformance with the established water quality standards
(TTBS, WHO) or with the maximum allowable levels of fecal coliform bacteria for a specific water body
e.g Table 1. The Feacal coliform (FC) is a subset of the coliform group.

Table 1. Acceptable coliform standards (colonies/100mLwater sample)

Drinking water
Swimming (pools)
Boating (lakes etc.)
Treated sewage effluent should not exceed

1 Total coliform
200 Feacal coliforms
1000 Feacal Coliforms
200 Feacal Coliforms

Principle of the MF method for Total and Feacal Coliforms

The membrane-filtration method is used to bacteriologically assess a water sample quantitatively rather
than qualitatively. A measured volume of sample is filtered through a cellulose membrane filter of pore
size 0.45 micron. Any microorganisms in the sample will be retained on the filter which is transferred to
a sterile Petri dish containing the growth media- either M-Endo agar (for Total Coliform) or MFC agar
(for fecal coliforms). The Petri dish is incubated for at least 16 hrs at 35.5oC (M-endo) and 44.5 oC
(MFC).

The appropriate conditions (temperature, moisture and time) will encourage the growth of coliforms while
suppressing the growth of all other microorganisms. Each microbe develops into a separate colony,
which can be observed with the naked eye identified by its characteristic color, and counted. The results
are calculated to give the number of coliforms in 100 mL sample.

Material
Membrane filters (0.45 um)
Petri dishes, with growth media - (MFC and M-Endo)
Graduated cylinders -100mL
Dilution water
Alcohol burner
Vacuum pump with filtration apparatus
Incubator @ 35 o C - for Total Coliform ;
Water bath @ 44 o C for Fecal Coliform
Plastic bags
Transfer forceps

Samples
Use the following samples for THIS TEST ONLY
Sample AWater from the laboratory tap
Sample B River water treated with household bleach
Sample C River water untreated
At times the degree of pollution in a water sample makes it difficult to accurately determine the actual
number of organisms present. In that case, a serial dilution (shown below) is used to ensure that the
number of colonies on the membrane filter does not exceed 20-80 colonies.
The serial dilution procedure should be performed on sample C only

SERIAL DILUTION PROCEDURE

Using a CLEAN I mL PIPET for each dilution
Pipette 1mL sample C into dilution bottle 1Pipette 1mL from bottle 1 into dilution bottle 2 Pipette 1mL from bottle 2 into dilution bottle 3 -

Test the samples in the following order and volumes

1. Sample A - 100 mL
2. Sample B - 25 mL
50mL
3. Sample C - bottle 3 - 10 mL
bottle 2 - 1 mL and 10 mL
bottle 1 - 1 mL and 10 mL

10

(1/100)
(0.01/100)
(0.0001/100)

Procedure
Total Coliform Test
1. Assemble the membrane filter apparatus as demonstrated
2.
3.
4.
5.
6.
7.
8.
9.

Using the forceps insert the MF (grid side up)

Shake the sample to be tested vigorously, then, measure the volume to be tested.
Top up the cylinder to 100 mL with sterile water, pour the contents into the filter funnel and suction.
Rinse the cylinder and the sides of the funnel with approx. 50 mL of the sterile dilution water.
Suction the MF until dry, then using forceps, immediately transfer the MF to a labeled Petri dish
prepared with M-Endo agar (identified).
Incubate the inverted petri dish at 35 o C for 16-24 hours.
Remove the Petri dish from the incubator after 16-24 hrs. Count only those colonies with a greengold metallic sheen.
Report the calculated number of colonies for 100 mL of sample.

Fecal Coliform Test

1. Immediately after doing the TC test on a sample repeat steps 2 to 5 above.
2.
3.
4.
5.
6.

Transfer the MF to a Petri dish with MFC media (as identified)

Enclose the Petri dish in a plastic bag and seal.
Rack the sealed bag and submerge the rack in a water bath at 44 o C for 16-24 hours.
After 16 to 24 hours, remove the Petri dishes from the water bath and carefully count only the blue
colonies.
Calculate and report the colony count for 100 mL of sample as before

Colony Counting
After incubation, there may be a growth of micro-organism, on the MF. The fecal coliform colonies
appear blue and the total coliforms will appear metallic green while non-fecal coliform colonies will
appear gray or cream. A valid dilution is the one which provides 20 to 60 colonies per filter. A counts for
each dilution must be recorded on the laboratory data sheet.
NOTE: Massive, uncountable growth over the entire surface of the MF should be recorded as TNTC (too
numerous to count).
Calculations
# of colonies counted

Coliform colonies for 100 ml of sample =

X 100
volume of sample filtered

11

2. Jar Test
Turbidity in water is caused by the colloidal particles which impede the passage of light. Turbidity is
measured in NTU - Nephelometric Turbidity Units (see figure). Turbidity over 5 NTU is noticeable and
usually unacceptable.

Jar testing is a common laboratory procedure done to simulate the coagulation, flocculation and
sedimentation processes used to remove turbidity from water. It is used to determine the optimum
coagulant dose to be used to treat particular water or wastewater on a laboratory scale in order to predict
the requirements for a large treatment plant
The untreated river water sample provided is to be used for the Jar Test.
Procedure
1. Put 500 mL of the river water sample provided, in each of six (6) 1L beakers.
2. Use - Calum Valum = Cjar Vjar to calculate the appropriate volumes of 5000 mg/L alum solution
required to give concentrations of 0 to 90 mg/L alum in each jar, as labeled
3. Add the appropriate volumes of the alum provided to each of the six (6) beakers
4. Rapid mix at 100 rpm for 1 min after the alum addition.
5. Reduce the speed to 20 rpm without stopping the process.
6. While mixing compare the floc sizes and characteristics of floc formation in each beaker.
7. After 7min stop the mixing, remove the paddles and allow settling for 7min.
8. Pour off the supernatant (liquid at the top of each beaker) into the small beakers provided
without disturbing the settled floc.
9. Measure the turbidity and pH of each supernatant.
10. Identify the optimum coagulant dose on a graph of the final turbidity and pH
measurements.

Turbidity measurement
Apparatus/Reagents
Jar test apparatus
Aluminum Sulphate Solution
Turbidimeter
Sample cells, lens tissue
Distilled water

12

Procedure
1. Gently pour the sample up to the measurement line (approx. 30 mLs) in a clean cell
2. Cap and wipe the cell with tissue paper.
3. Place in the cell compartment of the Turbidimeter, close the lid and allow the reading to stabilize
(approx. 1-2 mins).
4. Record the turbidity value on the instrument display.
5. Repeat the procedure for each sample.

3. Source Determination
A Source determination test is very often used to determine the source or origins of a water leak or an
unidentified body of water.
For this test you are provided with three (3) treated water samples, each from a different water
source/ location. Use the results of the following 5 tests to determine the source of each sample.

Test 1. pH
pH indicates the nature (acidic, alkaline and neutral) of a sample. The results can also be used to
determine the possible presence of contaminants such as industrial or chemical wastes in water supplies.
Two methods can be used to measure pH.
1. Visual - pH strips
2. Electrometric - pH meter
Using the visual method, determine the pH of sample X, Y & Z provided
Materials
pH papers
pH meter with electrodes
100 mL beakers
Distilled water
Procedure
1. Immerse the paper in the sample and remove it after 30sec.
2. Compare the color of the paper to the scale of colors printed on the packet as shown in the figure.
3. Record the matched pH value.

13

Test 2. Chlorine Residual

Chlorination of water supplies is done primarily to destroy or deactivate disease-producing
microorganisms. The chlorine residual is the chlorine that remains in the water supply to provide longterm disinfection, once the Chlorine Demand has been satisfied.
Determine the residual chlorine levels of samples X, Y & Z.
Apparatus/Reagents
HACH Colorimeter + 10 mL tubes
DPD reagent packets for Total and Free Residual chlorine
Procedure
1. Fill the two 10 ml cells /tubes to the 5ml mark with sample
2. Add the contents of the DPD Free chlorine packet to one tube and the contents of the DPD Total
Chlorine packet the other.
3. Cap and shake both tubes for 30 seconds
4. For Free residual chlorine - 1 minute after adding the DPD, wipe excess liquid and fingerprints
from the outside of the tube and put it in the cell holder of the HACH colorimeter,
5. Cover with the instrument cap and press read/ enter the instrument will show ------ followed by
the Free Residual Chlorine results in mg/l (ppm)
6. For Total Chlorine - 3-6 minutes after adding the DPD reagent, wipe excess liquid and
fingerprints from the sample cell, put it in the cell holder of the HACH colorimeter,
7. Repeat step 5.
8. Record the Free & Total Chlorine Residual in mg/L (ppm)
9. Repeat procedure for all 3 samples

Test 3. Hardness
Hard Water does not readily lather with soap. Generally, it is as satisfactory for human consumption as
soft waters but hardness is an important factor in industry because of tendency to form a scale in boilers,
water heaters and distribution systems. Water hardness varies considerably from source to source and
excess hardness can usually be removed by a combination of chemical and physical water treatment.
Determine the Hardness of samples X, Y & Z
Apparatus/Reagents

Burette, pipettes
125 ml conical flasks
25 ml measuring cylinder
Distilled water

Erichrome black T indicator

Ammonia buffer
EDTA

14

Procedure
N.B Complete titration within 5mins after adding the indicator.
1.
2.
3.
4.
5.

Fill the burette with the EDTA

Measure 25 mLs of the sample. Transfer volume to a conical flask.
Add 1 mL buffer solution, 5 drops of the indicator and swirl flask to mix.
Titrate from a purple to the first permanent blue end point.
Record all titer values and repeat procedure

Calculations
Titre value x 1000

Hardness as mg CaCO3/L =

vol.of sample tested

Test 4. Alkalinity
Alkalinity is the capacity of water to neutralize acid. In natural waters, the major contributors to
alkalinity are hydroxides, carbonates and bicarbonates. Alkalinity measurements are used to control
treatment processes and many chemicals used in water treatment can also cause an alkalinity change.
Total alkalinity (T) = (HCO3) + (CO32) + (OH)
Phenolphthalein alkalinity (P) = (CO32) + (OH)
The following table can be used to calculate the different forms of alkalinity as mg/L CaCO3

Table 2: Alkalinity forms

Result of Titration
P=0
2p < T
2p = T
2p > T
P=T

Apparatus/Reagents
250 ml conical flasks
burette, pipettes
100 ml measuring cylinder
Distilled water

Hydroxide
(OH)
0
0
0
2p - T
P

Carbonate
( CO32)
0
2P
2P
2(T-P)
0

Bicarbonate
( HCO3-)
T
T-2P
0
0
0

Screened Methyl Orange

phenolphthalein indicators
0.02N Sulphuric acid
Sodium Thiosulphate solution

15

Procedure
1. Fill the burette with 0.02N sulphuric acid.
2. Transfer 100 ml of the water sample to a conical flask.
3. Add 2 drops of the sodium thiosulphate solution and mix to remove any residual chlorine which
would interfere with indicator response.
4. Add 5 drops of phenolphthalein indicator.
5. If a pink colour develops titrate slowly until the sample becomes colorless and record the volume
of acid used
6. If no pink colour develops continue with (7)
7. Add 3 drops of screened methyl orange indicator to the same sample
8. Titrate slowly until the first grayish colour change appears.
9. Record all titer values and repeat procedure.
Calculations
Titre value x 0.02 x 50000

Alkalinity (Tor P) mg CaCO3 /L =

vol.of sample tested

Test 5. Chloride
Chlorides in natural waters can be attributed to the dissolution of salt deposits; discharges of effluents
from chemical industries; oil well operations and sea water intrusion in coastal areas. A chloride
concentration of 250mg/L may cause a salty taste in water depending on the predominant ions present.
Additionally, high chloride content may harm metallic pipes and structures as well as plants

Apparatus/ Reagents
Burette, pipettes
125 ml conical flasks
25 ml measuring cylinder
Distilled water

Diphenyl carbazone indicator

Nitric Acid
Mercuric nitrate titrant

Procedure
1.
2.
3.
4.
5.
6.
7.

Fill the burette with the Mercuric Nitrate

Transfer 25mls of the sample to a conical flask.
Add 5 drops of indicator and swirl flask to mix
Add 2 mls of Nitric acid, swirl flask again to mix
Titrate from a light yellow to a permanent deep purple end point.
Record titer values
Record all titer values and repeat procedure

Calculations
Titre value x 500

Chloride as mg/L Cl- =

16

vol.of sample tested

Discussion
Analyze ALL your results
Indicate whether samples A, B & C were bacteriologically safe or unsafe. Reference and cite the
appropriate Water Quality Standards.
Include a brief description of your observations and each stage of the jar test procedure.
Include a brief description of the processes used to make ground, surface, and sea water potable.
Identify the source of samples X Y& Z with justification for your choices.
Include the sources of error and limitations for each test.

General Questions
1. Using Table 2, determine the different forms (T, P, HCO3, CO32, and OH) of alkalinity in samples
X, Y & Z.
2. Provide a rationale for testing water supplies for coliform bacteria and show how you would
measure0.001 mL of a very contaminated water sample for testing.
3. What is the Water quality Index WQI? Use the Chart below to determine the Q value for your
fecal coliform results.

Water Quality Index - WQI

Fecal coliform (FC): colonies/100ml

Note: if FC>100,000, Q=2.0

17

4. Why is it important to measure and limit the levels of turbidity in water courses? What may be
causes of high turbidity in ground water and how can it be removed from in order to make the
water potable?
5. Indicate the similarities and differences in the graphs shown below and your jar test graph.
Determine the optimal alum dose for the three plots?

Jar Test Graphs

1.

Tubidity (NTU)

30
25
20
15
10
5
0
0

10

15

20

25

30

Alum dose (mg/L)

Settled Turbidity as a Function of Alum Dose at 30 rpm

2.

18

35

ACTIVITY 2 Wastewater Analysis

INTRODUCTION
Wastewater water which has been used for many different purposes. It often includes fecal waste, food,
oils, soap/ detergents, toxic chemicals and many other constituents. There are many types of wastewater
domestic, industrial, agricultural, process, institutional. Sewage is wastewater which is contaminated
with fecal matter but the term is often used to describe all wastewater.
Wastewater is usually conveyed in a combined sewer and treated at a municipal wastewater treatment
plant or an (on site) septic tank system. The treated wastewater (effluent) is usually discharged into a
receiving water course.

Typical Flow Diagram for an Extended Aeration Wastewater Treatment Plant

Source: http://img.docstoccdn.com/thumb/orig/4214411.png

A process is usually designed to treat a particular type of wastewater e.g domestic wastewater is readily
treatable in a municipal wastewater treatment plant using extended aeration whereas that process may not
be able to treat industrial wastewater containing high percentages of toxic chemicals, organic materials
and solid organic material or FOG residues.
Storm water or run-off is another type of wastewater which will usually go into a domestic wastewater
treatment plant, a receiving water course or a retention pond. Although storm water is usually low in
pollutants, in large volumes it can interfere with the operational efficiency of a wastewater treatment
plant.

19

Objectives
-

To introduce students to the most common laboratory tests that are used to assess the efficiency
of a wastewater treatment plant
To assess the quality of wastewater effluents that are discharged into receiving water courses and
to compare the effluent quality to Sandards
To demonstrate the standard procedures/methods, tools, apparatus and equipment used in an
Environmental Laboratory.
To illustrate the limitations of the methods/procedures used to assess WW quality
To provide experience in analyzing results from laboratory tests.

Learning Outcomes
At the end of this exercise the student will be able to:
Identify the apparatus required to conduct some experiments on WW
Perform experiments in accordance with written procedures/ methods / instructions
Obtain readings and measurements from standard laboratory equipment with minimum error
Manipulate and interpret laboratory data and use the results to infer wastewater quality
Determine the performance efficiency of a wastewater treatment plant
Observe at practice laboratory safety

ANALYSIS
For this lab you are provided with Influent and Effluent samples taken from wastewater treatment Plants.
The following tests are to be performed on the samples provided.
1- pH
2- Settleable Solids (SS)
3- Suspended Solids (TSS)
4- Dissolved Oxygen (DO)
5- Biochemical Oxygen Demand (BOD)

Test 1 pH
pH is the measure of hydrogen ion activity in the given sample. The measurement indicates whether the
WW is acidic, alkaline or neutral. Two test methods can be used: 1. Visual pH paper and
2. Electrometric - pH meter
Use both methods to determine the pH of the samples provided
Materials
pH papers
Calibrated pH meter with electrodes
100 mL beakers
Distilled water

20

Procedure
a. Using pH paper.
Immerse the pH paper in the sample and hold it for about 30 secs. Do not shake it to dry. Match
the colors on the paper to the scale of colors provided. Record the value of the matched pH
value.
b. Using the pH meter
1. Rinse electrodes several times with the distilled water.
2. Rinse the beakers with a little of the sample to be measured then fill it with approx. 100mL
3. Immerse the electrodes in the sample.
4. Use the magnet to slowly agitate the sample while allowing the meter to stabilize
5. After 2-3 minutes record the pH value.
6. Repeat the procedure for all samples.

Test 2 - Settleable Solids (SS)

The Settleable solids test is used to measure the volume of solids settling from the wastewater after a
specific time period. SS can be used to:- indicate the quality of the influent;
- establish the settling behavior of the wastewater and
- estimate the sludge volume that will accumulate, over time, in the clarifier, sedimentation tanks
and ponds.
Apparatus
Imhoff cone and holding rack
Stirring rod and Timer
Procedure
1. Thoroughly rotate the sample to mix.
2. Immediately after mixing, fill the Imhoff cone to the 1 liter mark with the sample.
3. Allow settling for 45min. Then agitate by gently lifting and rotating the cone.
4. Allow settling for a further 15mins
5. At the end of one hour settling time, record the volume of solids in the Imhoff cone.

Calculations
Report the volume of solids settled as: Milliliters of settled solids per liter of wastewater mL/L

21

Test 3 - Total Suspended Solids (TSS)

Total suspended solids (TSS) include all particles which will not pass through a filter. Suspended solids
are present in sanitary wastewater and many types of industrial wastewater. The amount of suspended
solids will usually increase with the degree of pollution. The measurement is mainly used to assess
whether the waste effluent from a WWTP conforms to Standards for effluent quality before it is
discharged.
Apparatus
Glass-fiber filter discs (GFC- 934AH paper)
Aluminum containers
Filtration apparatus
Analytical balance

Drying oven (103o - 105o)

Large tip pipettes
Distilled water

Procedure
1. Determine the mass of filter paper and aluminum dish (M1)
2. Place the filter disc on the filtration apparatus, rinse with a small portion of distilled water and
suction dry (no more drips).
3. Pour approx. 1 L of sample into a beaker and slowly mix using a magnetic stirrer.
4. While mixing, pipette and filter 4 - 25mL volumes of the sample taken from midway the total 1L
volume.
5. Rinse sides of apparatus with small portions of distilled water and suction the filter to dryness.
6. Transfer the filter back to the aluminum dish and dry it in an oven at 103 -105o C for 20 mins to 1
hour.
7. Cool the dish and filter paper, in the desiccator, for approx. 20 min
8. Re-weigh and record weight (M2) to a constant weight.

Calculations
TSS g/mL =

(M 2 M 1 )g
(volume of sample filtered)mL

Report results in mg/L

Test 4 - Dissolved Oxygen (DO)

Dissolved oxygen (DO) in water is a common indicator of the health of a water body. If a system uses
more oxygen than what is added the DO levels decline and sensitive aquatic species may move away,
weaken or die. DO levels in water bodies should therefore be maintained above 4.2 mg/L. DO levels in
water can be determined using either the classical Winklers (idometric) titration or the membrane
electrode method.

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Principle of the Electrode Method

The electrochemical method requires a DO meter which is used to
measure the pressure of oxygen in the water. The cathode/anode
electrode which is filled with electrolyte solution has a gas permeable
membrane (see figure). The membrane permits oxygen to diffuse
into the electrolyte solution. A partial pressure is then created across
the cathode.

Principle of the Winklers Titration

In Winklers titration, a DO bottle is completely filled with the water to be tested. Chemical reagents,
added in excess, interact with oxygen to form a floc which is acidified to release the DO. Sodium
thiosulphate (the titrant) is used to neutralize the acid and the amount needed is proportional to the
amount of DO in the sample. The volume of titrant used is reported in mg/l. Any delay between the time
of sample collection and testing may result in the DO being altered by atmospheric oxygen. This method
may be more accurate since it allows the DO to be fixed in the field.

Materials
Burette, pipettes,
measuring cylinders
250 mL beakers,
250 mL Erlenmeyer flasks
300 mL BOD bottles

Manganous Sulphate - reagent A

Alkaline Azide Iodide - reagent B
Concentrated Sulphuric acid
Starch solution
Sodium Thiosulphate (titrant)

Both the Winklers (idometric) titration and the meter/electrode method will be used to measure the DO
in the samples provided

Winklers (Idometric) Titration Method

Exercise caution with the reagents. Refer to the MSDS sheets (Appendix 1) for safety information
Procedure
Step 1 - DO fixing
1. Carefully fill the 300 mL BOD bottles provided with the samples, until the bottle overflows.
2. Use the bottle cover to gently tap on the bottle to remove any air bubbles trapped in the liquid,
stopper and then rinse the outside of the bottle under the tap,
3. Add 2 mL reagent A to each bottle by placing the delivery pipette just below the level of the
sample.
4. Replace the stopper, dump excess displaced liquid and rinse the outside of the bottle again.
5. Add 2 mL reagent B to each sample in the same manner as (3).
6. Repeat step 4.
7. Gently invert each bottle several times to mix sample and reagents.
8. Allow the floc formed to settle to approx. the sample volume.

23

9. Repeat the inversion to mix and allow settling again.

10. After the second settling, carefully add 2 mL Conc. Sulphuric acid to each bottle while holding
the pipette just above the surface of the sample.
11. Cover bottle and invert until the floc dissappears.
Step 2 - Titration
12. Use a measuring cylinder to transfer 201 mLs of the sample to a conical flask.
13. Use the Sodium Thiosulphate to titrate against the sample in the flask until the yellow almost
disappears. Stop and do not record the burette reading.
14. Add 2 mL of starch to the sample, mix well to develop a blue color and continue titrating to a
colorless end point.
15. Record the final burette volume.
16. Repeat the titration for all samples
DO in mg/l = Titrant volume in mls

DO Meter / Electrode Method

Procedure
1. Place the probe in the sample.
2. Put on the probe to self-stir
3. Allow time for the temperature and dissolved oxygen readings to stabilize.
4. Read the dissolved oxygen and temperature off the meter when the asterisk appears as shown in
the figure below

Test 5 - Biochemical Oxygen Demand (BOD)

The 5-day BOD (BOD5) is the most widely used indicator of organic pollution in water and wastewater.
BOD gives the relative oxygen-depletion effect of contamination and pollution loading within a system
since it measures the oxygen demand of any biodegradable pollutants in water/wastewater. A major
disadvantage of the BOD test is the length of time (3- 5 days) it takes to obtain results.

24

Principle of the method

A special airtight 300ml (BOD) bottle is filled with varying amounts of wastewater which is diluted with
oxygenated dilution water. The initial DO is measured and the sample is incubated at approx. 20o C for 5
days (standard) or 27o C for 3days. The final DO is measured after the incubation period and the BOD
is calculated from the DO depletion.
Sample size/ Dilutions
Generally, the oxygen demand of most wastewater is greater than the amount of oxygen available in a
300ml bottle. The wastewater must therefore be diluted in order to ensure that sufficient oxygen is
present in the sample bottle for the incubation period. Generally 3 dilutions are used
The following is used to determine the dilutions which should ensure valid BOD results are obtained:1. The DO of the original, undiluted sample.
2. The sample source (raw sewage, sewage effluent, river water, storm water).
3. Previous BOD records for the same or a similar source.
4. The COD of the sample if available (this test can be done in 2- 3 hours)
A good BOD dilution should use at least 2mg/L of oxygen over the incubation period and leave a
residual of at least 1mg/L.
Materials
50mL graduated (straight) pipets,
Measuring cylinders (100mL, 250mL)
500mL volumetric flasks
DO meter with probe
BOD incubator at 35.5 or 27oC
300mL DO bottles and plastic sealing cups
Dilution water aerated distilled with all reagents added.
Procedure
1. Fill the BOD bottles provided with each of the three samples (Influent, effluent and pond)
2. Using the DO meter, measure the initial DO of the samples and record the values
3. Prepare sample dilutions using the instructions below.
1. Influent sample
2. Effluent sample

2%, 3%, 5%
20%, 30%, $0%

N.B: These dilutions may be adjusted depending on the nature of the sample on the day of the test.
4.
5.
5.
5.
6.

Convert % dilutions to volumes in 300 ml and put the volumes determined into the BOD
bottles provided.
Carefully fill the DO bottles to the neck with dilution water provided.
Use the DO meter to measure the initial DO value (I-DO) of each dilution.
Record the BOD bottle numbers, sample dilutions and I-DO readings.
Replace any dilution water displaced from the BOD bottle, ensure that no air bubbles are trapped
inside and stopper tightly.

25

7.

Thoroughly rinse the outside of the bottle, form a seal at the top with water and snap on the plastic
cap provided.
8. Prepare a dilution water blank (dilution water without sample)
9. Incubate all the samples at 27oC for 3 days
10. Measure the Final DO value (F-DO) after the 3 day incubation period,
11. Calculate the BOD3 using the equation below.

Calculations
BOD3, mg/L =

Where -

D1 D2
x 300
V

D1 = DO of diluted sample before incubation, mg/L

D2 = DO of diluted sample after 3d incubation at 20oC, mg/L
V = calculated volume (ml) of sample used in the test

Note: If, after 3 days, the final DO is less than 1mg/L the BOD cannot be determined. Why?
If there are no obvious anomalies in the results, report an average of the three calculated, BOD values as
the final BOD in mg/L.
In this exercise, the dilution water blank is being used as a check on the quality of the dilution water and
the overall cleanliness of the glassware. It is therefore not necessary to correct the calculations for the DO
depletion in the blank. If however, the DO depletion for the blank is extremely high and it is clear that
the test might have been affected by the quality of the dilution water, the results will be disregarded.

26

Discussion
-

Interpret and discuss the results from all 5 tests.

Compare the two pH methods (pH paper and pH electrode) and the two DO methods (Winklers
titration and Meter /electrode). Discuss the validity, practicality and degree of accuracy of either
method.
Discuss the possible sources of error.
Compare results to Standards for Effluent Quality WW discharged into a receiving water
Calculate efficiency and discuss the plant performance from an engineering stand point.

General Questions
1.

Wastewater effluent that is discharged into the environment must be in compliance with certain
standard values. What does compliance mean and what are the Standards for Trinidad & Tobago?

2.

What factors control the DO levels in a stream? Wastewater from a food processing plant with an
extremely high BOD is discharged into a low flow stream every day. What will be the long term
and short term effects on the stream?

3.

Compare aerobic and anaerobic wastewater treatment.

4.

Recommend engineering interventions for improving the performance and efficiency of a WW

treatment plant.

5.

a.
b.

Determine the 1- day BOD and the ultimate first stage BOD for a wastewater with a 5 - day
20oC BOD of 725 mg/L. The reaction constant k (base e) = 0.23d-1.
Calculate the BOD5 if the test was conducted at 25oC and the samples were incubated for three
(3) days?

27

Activity 3 Field Trip

A visit to the Caroni Water Treatment Plant in Piarco and the Beetham Wastewater
Treatment Plant in Port- of Spain will be conducted. The field trip provides a great opportunity
to understand the lecture notes. At the end of the trip you should have a very good idea of the
quality of the influent (raw water in the case of water treatment), the catchment areas from which
it was derived, and the reason for the treatment processes employed to produce the required
effluent (product). Pay attention to the processes and the technologies used for ensuring
consistent quality

The Caroni Arena Water Supply System (CAWSS)

provides water to the North, West, Central and Southern
regions of Trinidad. The Caroni Water Treatment Plant
treats water from the Caroni River. The Reservoir was
commissioned in 1981; the first (old) plant in 1981 and
the second (new) plant in 2000. The system is comprised
of the Arena dam, reservoir and pump storage complex
on the Arena tributary of the Caroni River; the Caroni
Water Treatment Plant; transmission pipelines and
secondary pump stations and storage reservoirs that store
the treated water for distribution to various areas.
Arena Dam - CAWSS
The New Beetham Wastewater Treatment Plant is the
largest wastewater treatment facility in the Caribbean.
The plant was commissioned in 2004. The 180 ML/d
activated sludge plant services Port of Spain and its
environs. It is constructed in a mangrove swamp and
produces a high quality effluent which is suitable for
discharge into the environmentally sensitive Caroni
Swamp.

.
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Health and Safety

The plants are environments in which a significant number of persons work. Some are actively
involved in the operations to produce the product; others, such as the security officers and the
janitors although not directly involved in the production may be on the plant for 8 hours at a
time. Observe the environments of the plants and identify the health and safety hazards that are
inherent in their operations and then find out the measures, both procedural and structural, that
have been put in place, or should be put in place, to minimize the risk.
Here are some possible hazards. The list is not complete:

Exposure to chemicals ( water treatment)

Exposure to contamination ( wastewater)
Danger of falling into tanks, of great depth, with and without water;
Ascending and descending ladders and staircases;
Vehicular traffic to and from the location;
Overhead and moving equipment;
Dust; Noise;
Generally unsafe environment.

Sustainability
Over the years, Civil engineers have boasted of their capability to treat any water or wastewater
to the required standards. This gave little consideration to the resources required to do so.
Therefore, low on the list of priorities was the protection of the watersheds to improve the
quality of the raw water because it was felt that the required quality could have been achieved by
increased chemical dosages. In the same vein, not much concern might have been given to the
energy required for running the plants.
Now we are aware of the importance of designing sustainable systems and that if we use that
approach in our practice then we will make more efficient and effective use of earths resources
and so increase the chances that future generations will have sufficient resources to meet their
needs.
As you tour the two treatment plants consider in the case of water treatment the raw water
quality and depletion, on one hand, and in the case of wastewater treatment the volume of
effluent wastewater produced which could be reused. Determine the processes, in terms of the
chemical requirements, the size of the tanks, and the energy required for running both plants.

More Information on the operation of both plants will be provided by WASA personnel

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Field Trip Report Format

Cover (Title) page

Same format as the lab reports [2]

Abstract

Provide a short (one paragraph) summary of the entire report. [3]

Objectives

State, in your own words, the objectives of the exercise. [2]

Introduction

Address the environmental/ health importance of treating wastewater and water [3]

Theory

Provide a brief summary of the theoretical underpinnings of both treatment

processes. Provide proper citation for all information referenced [5]
Include the under mentioned key words and terms to describe the actual treatment
process used on both plants and the significance of each stage.

Treatment
processes

Wastewater treatment - head works/ wet well; Influent /Grit screening;

Bioreactors / RAS/WAS/ anoxic zone / aerobic; Clarifier; UV treatment /
disinfection; Sludge handling [10]
Water Dam; Raw intake head works / raw water pumps; screening;
coagulation/ flocculation; sedimentation/ sludge handling ; filtration;
disinfection; distribution/ transmission system [10]
Include Flow diagrams for both treatment processes.

Discussion

Discuss your observations in terms of the following:Engineering devices and operations used on each plant
Health and Safety practices and risk management
Sustainability
Quality assurance (QA) and quality control (QC)
Compare your findings with those given in lectures or other references. Further,
discuss the degree of confidence you can place in the plant operations [10]
Avoid the temptation to repeat what you said in your introduction

Conclusion

Summarize the key findings and whether your stated objectives were achieved [3]

References

Cite and reference all sources used (including websites) using the proper
(Chicago) style format [2]

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References
1.
2.
3.
4.
5.
6.

(AWWA, APHA, WPCF) Standard Methods for the Examination of Water and Wastewater.
Viessman W and Hammer M.J., Water Supply and Pollution Control.
Peavy H.S, Rowe D.R, Tchobanoglous G, Environmental Engineering
Sawyer C.N, McCarty P.L, Parkin G. F, Chemistry for Environmental Engineering.
Relevant web sites
Links to Material Safety Data Sheets (MSDS) below.
Substance

Web page

MFC Agar

http://www.oxoid.com/pdf/msds/EN/MM0747.pdf

M-endo Agar

http://msds.egeneralmedical.com/em1.11277.0500.pdf

Aluminum Sulphate

http://www.sciencelab.com/msds.php?msdsId=9922861

DPD - n n-diethyl-pphenylenediamine sulfate

http://www.nwmissouri.edu/naturalsciences/sds/n/N%20NDiethyl-p-phenylenediamine%20sulfate%20salt.pdf

Erichrome black T indicator

https://www.google.tt/?gws_rd=ssl#q=eriochrome+black+t+indica
tor+msds

Ammonia buffer

http://www.labchem.com/tools/msds/msds/75517.pdf

EDTA

https://lifesciences.byu.edu/Portals/6/docs/EDTA.pdf

Screened Methyl Orange

http://www.lovibondmsds.co.uk/msds/AS-K27629KW_KS537_(GB).pdf

phenolphthalein indicator

http://www.btps.ca/files/PDF/MSDS/Phenolphthalein_Indicator_S
olution_528.00.pdf

Sulphuric acid

http://www.sciencelab.com/msds.php?msdsId=9925146

Sodium Thiosulphate

http://www.massasoit.mass.edu/assets/pdf/msds/sodium%20thiosu
late%20pentayhydrate.pdf

Diphenyl carbazone
indicator
Nitric Acid

http://www.riccachemical.com/Technical-Support/MSDS/2600

Mercuric nitrate

http://www.labchem.com/tools/msds/msds/75496.pdf

Manganous Sulphate

http://www.labchem.com/tools/msds/msds/75541.pdf

Alkaline Azide Iodide

http://www.labchem.com/tools/msds/msds/LC10670.pdf

Starch solution

http://www.sciencelab.com/msds.php?msdsId=9926918

http://kni.caltech.edu/facilities/msds/Nitric_Acid.pdf

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