muneeb manual
muneeb manual
muneeb manual
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INDEX
Activity Page no.
Water Sampling Methods for Lab Analysis 3
2
Water Sampling Methods for Lab Analysis
3
Meaning of Water Quality Analysis:
Water quality standards are put in place to ensure the efficient use of water for a
designated purpose. Water quality analysis is to measure the required parameters of
water, following standard methods, to check whether they are in accordance with the
standard.
The methods that will be followed will determine the type of bottles used. For example,
samples for metals’ analyses are usually collected in plastic bottles, while analyses for
volatile organics and pesticides are collected in glass containers. Bottles used to collect
samples for bacteria should be sterilized. Certain analysis like volatile organics and radon
require vials that are to be filled leaving no head space, which keeps these analytes dissolved
in the water, preventing them from escaping into the air. Additionally, some analyses require
samples to be collected in amber colored bottles. These darker bottles are for analytes that
break-down in sunlight, which helps keep these contaminants from breaking down while in
transit to the laboratory for analysis. The size of the container is important to ensure enough
sample to run the analysis needed.
Integrated sampling:
Integrated samples are a mixture of grab samples collected from different points
simultaneously and mixed in equal volumes.
Sample Preservation:
There is usually a delay between the collection and analysis of a sample. The nature of the
sample can be changed during this period. Therefore proper preservation is required in the
way to laboratory after collection, and in the laboratory up to when analysis starts.
Complete and unequivocal preservation of samples, whether domestic wastewater, industrial
wastes, or natural waters, is practically impossible as because - complete stability for every
constituent never can be achieved.
At best, preservation techniques only retard chemical (especially, hydrolysis of constituents)
and biological changes that inevitably continue after sample collection. No single method of
preservation is entirely satisfactory; the preservative is chosen with due regard to the
determinations to be made.
Commonly used preservation methods are - pH control, chemical addition, the use of amber
and opaque bottles, refrigeration, filtration, and freezing.
Assignment:
Collect your water sample from the location as instructed by the course teacher in the class. Follow
the standard procedure during sample collection and preservation. Prepare a sample collection report
(on A4 offset paper) describing details of sampling method (e.g. location, weather condition, details
of surrounding features etc.) and also provide some pictures taken at the collection site.
6
Experiment 1
Determination of pH in water
7
Introduction:
The term pH refers to the measure of hydrogen ion concentration in a solution and defined as
the negative log of H+ ions concentration in water and wastewater
1.1
Where {H+} is the concentration (or activity) of hydrogen ion (or photon) in moles per liter
(M).
Water dissociates to form hydrogen ion (H+) and hydroxyl ion (OH-) according to the
following equation:
= 1.2
1.3
But, since concentration of water is extremely large (approximately 55.5 mol/L) and is
diminished very little by the slight degree of ionization, may be considered as a constant and
its activity is taken as 1.0. Thus Eq. (3) may be written as:
1.4
The values of pH,0 to a little less than 7 are termed as acidic and the values of pH a little
above 7 to 14 are termed as basic. When the concentration of H+ and OH- ions are equal then
it is termed as neutral pH.
Environmental significance:
Determination of pH is one of the important objectives in biological treatment of the
wastewater. In anaerobic treatment, if the pH goes below 5 due to excess accumulation of
acids, the process is severely affected. Shifting of pH beyond 5 to 10 upsets the aerobic
treatment of the wastewater. In these circumstances, the pH is generally adjusted by addition
of suitable acid or alkali to optimize the treatment of the wastewater. pH value or range is of
immense importance for any chemical reaction. A chemical shall be highly effective at a
particular pH. Chemical coagulation, disinfection, water softening and corrosion control are
governed by pH adjustment.
Lower value of pH below 4 will produce sour taste and higher value above 8.5 a bitter taste.
Higher values of pH hasten the scale formation in water heating apparatus and also reduce
the germicidal potential of chlorine. High pH induces the formation of tri-halomethanes,
which are causing cancer in human beings.
8
Guideline:
According to American Public Health Association (APHA) , drinking water
standard for pH ranges from 6.5 to 8.5.
Principle:
The pH electrode used in the pH measurement is a combined glass electrode. It consists of
sensing half-cell and reference half-cell, together form an electrode system. The sensing half-
cell is a thin pH sensitive semi permeable membrane, separating two solutions, viz., the outer
solution, the sample to be analyzed and the internal solution enclosed inside the glass
membrane and has a known pH value. An electrical potential is developed inside and another
electrical potential is developed outside, the difference in the potential is measured and is
given as the pH of the sample.
Apparatus:
1. pH meter
2. Beaker
Reagent:
1. Buffers Solutions of known pH value
Precautions
The following precautions should be observed while performing the experiment:
1. Temperature affects the measurement of pH at two points. The first is caused by the
change in electrode output at different temperatures. This interference can be controlled
by the instruments having temperature compensation or by calibrating the electrode-
instrument system at the temperature of the samples. The second is the change of pH
inherent in the sample at different temperatures. This type of error is sample dependent
and cannot be controlled; hence both the pH and temperature at the time of analysis
should be noted.
2. In general, the glass electrode is not subject to solution interferences like color, high
salinity, colloidal matter, oxidants, turbidity or reductants.
3. Oil and grease, if present in the electrode layer, should be removed by gentle wiping or
detergent washing, followed by rinsing with distilled water, because it could impair the
electrode response.
4. Before using, allow the electrode to stand in dilute hydrochloric acid solution for at least
2 hours.
5. Electrodes used in the pH meter are highly fragile, hence handle it carefully.
9
Procedure:
Three major steps are involved in the experiment. They are
1. Preparation of Reagents
2. Calibrating the Instrument
3. Testing of Sample
Steps:
Perform calibration of the pH meter using standard pH solutions. The calibration
procedure would depend on the pH range of interest.
In a clean dry 100 mL beaker take the water sample and place it in a magnetic stirrer,
insert the teflon coated stirring bar and stir well.
Now place the electrode in the beaker containing the water sample and check for the
reading in the pH meter. Wait until you get a stable reading.
Take the electrode from the water sample, wash it with distilled water and then wipe
gently with soft tissue.
Assignment
1. pH is one of the most important controlling factors for treatment and chemical analysis of water
and wastewater — explain.
2. Define pH in terms of hydrogen-ion (H+) concentration and hydroxyl-ion (OH-) concentration. An
increase in pH of one unit represents how much decrease in hydrogen ion concentration?
10
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
11
Experiment 2
Determination of Color in Water
12
Introduction:
Pure water should not pose any color. Color in water may result from the presence of natural
metallic ions (iron and manganese), humus and peat materials, plankton, weeds, and
industrial wastes. Impurities in water may exist either in the colloidal from or in suspended
state. Color caused by dissolved and colloidal substances is referred as "true color" and that
caused by suspended matter, in addition to dissolved and colloidal matters, is called "apparent
color" as it can be easily removed by filtration. Ground water may show color due to the
presence of iron compounds. The color value of water is extremely pH-dependent and
invariably increases as the pH of the water is raised. For this reason recording pH along with
color is advised.
Environmental significance:
Though presence of color in water is not always harmful to human but in most cases it is.
Even if the water is not harmful, aesthetically people do not prefer to use water with color.
Moreover, disinfection by chlorination of water containing natural organics (which produces
color) results in the formation of tri-halomethanes including chloroform and a range of other
chlorinated organics leading to problems which is a major concern in water treatment. So it is
important to limit the color of water for domestic supplies.
Guideline:
According to Bangladesh Environment Conservation Rules (1997), drinking water guideline
value for color is 15 Pt-Co Unit.
13
For dilution multiple methods, color is measured by successive dilutions of the sample with
color -free water until the color is no longer detectable comparing with distilled water. The
total dilution multiple is calculated and used to express the color degree.
3. Spectrophotometric method
The platinum-cobalt method is useful for measuring color of potable water and of water in
which color is due to naturally occurring materials. It is not applicable to most highly colored
industrial wastewaters. In the laboratory color of water is usually measured using
spectrophotometer which uses light intensity of a specific wavelength (455 nm). The color
test measures (inversely) an optical property of water sample which result from the
absorption of light of specific wavelength by the soluble color substances present in water,
Before measuring the color of water it is necessary to plot standard calibration curve for color
using different standard platinum-cobalt solutions of known concentrations within the range
of interest.
Figure 2.1: Optical property used in measurement of color in water using spectrophotometer
14
Apparatus:
1. Color Disk
2. Filtration system including filter paper, funnel, holder, beaker etc.
Reagent:
1. Standard potassium chloro-platinate solution
Procedure:
1. Prepare standard samples having color within a specific range by mixing different
concentration of standard potassium chloroplatinate solution with distilled water.
Using these samples to prepare a color calibration curve (absorbance vs. color
concentration) for the spectrophotometer.
2. Take 50-mL of filtered test sample in a beaker. Take 50-mL distilled water in another
beaker. Use this sample as blank.
3. Set the spectrophotometer to determine color concentration of the sample.
4. Put the blank sample inside the spectrophotometer cell and set the reading "zero''.
5. Bring out the blank sample and place the test sample inside the spectrophotometer
6. After a While the display will show the color concentration of the sample.
Assignment:
1. Define true and apparent color. Why true color is more important than apparent color?
2. Discuss the optical mechanism used in color measurement using spectrophotometer.
15
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
16
Experiment 3
Determination of Turbidity of Water
17
Introduction:
Turbidity is the technical term referring to the cloudiness of a solution and it is a qualitative
characteristic which is imparted by solid particles obstructing the transmittance of light
through a water sample. Turbidity often indicates the presence of dispersed and suspended
solids like clay, organic matter, silt, algae and other microorganisms. So in short turbidity is
an expression of the optical property that causes light to be scattered and absorbed rather than
transmitted in straight lines through the sample.
Environmental significance:
When the turbid water in a small, transparent container such as drinking glass is held up to
the light, an aesthetically displeasing opaqueness or milky coloration is apparent. The
colloidal material which exerts turbidity provides adsorption sites for chemicals and for
biological organism that may not be harmful. They may be harmful or cause undesirable
tastes and odours. Disinfection of turbid water is difficult because of the adsorptive
characteristics of some colloids and because the solids may partially shield organisms from
disinfectant. In natural water bodies, turbidity may impart a brown or other color to water and
may interfere with light penetration and photosynthetic reaction in streams and lakes.
Turbidity increases the load on slow sand filters.
The filter may go out of operation, if excess turbidity exists. Knowledge of the turbidity
variation in raw water supplies is useful to determine whether a supply requires special
treatment by chemical coagulation and filtration before it may be used for a public water
supply. Turbidity measurements are used to determine the effectiveness of treatment
produced with different chemicals and the dosages needed. Turbidity measurements help to
gauge the amount of chemicals needed from day-to-day operation of water treatment works.
Measurement of turbidity in settled water prior to filtration is useful in controlling chemical
dosages so as to prevent excessive loading of rapid sand filters. Turbidity measurements of
the filtered water are needed to check on faulty filter operation. Turbidity measurements are
useful to determine the optimum dosage of coagulants to treat domestic and industrial
wastewaters. Turbidity determination is used to evaluate the performance of water treatment
plants.
Turbidity in water may be caused by a wide variety of suspended matter suspended matter,
such as clay, silt, finely divided organic and inorganic matter, soluble colored organic
compounds, and other organisms. Under flood conditions, great amounts of topsoil are
washed to receiving streams. As the rivers pass through urban areas, the domestic and
industrial wastewaters may be added.
Guideline:
According to WHO standard 5 NTU is suggested as the turbidity limit for drinking water,
while 1 NTU is recommended to achieve the adequate disinfecting safety.
According to Bangladesh Environment Conservation Rules (1997), drinking Water standard
for Turbidity is 10 NTU (Nephelometric turbidity unit).
Principle:
Turbidity is based on the comparison of the intensity of light scattered by the sample under
defined conditions with the intensity of the light scattered by a standard reference suspension
under the same conditions. The turbidity of the sample is thus measured from the amount of
light scattered by the sample taking a reference with standard turbidity suspension. The
18
higher the intensity of scattered light the higher is the turbidity. Formazin polymer is used as
the primary standard reference suspension.
Because of the wide variety of materials that cause turbidity in natural waters, it has been
necessary to use an arbitrary standard. The original standard chosen was; 1 mg SiO2/L =1
unit of turbidity. The silica used had to meet certain specifications as to particle size. The
Jackson candle turbidimeter has been replaced by more reliable, sensitive, and easier to use
instruments that depend upon the principle of nephelometry. As a standard reference material,
Silica has been replaced by formazin polymer. The formazin suspensions were first calibrated
against the Jackson candle turbidimeter. The standard nephelometry procedure is now
reported in nephelometric turbidity units (NTU). Because the basic principles difference for
Jackson candle turbidimeter method and nephelometric method, results got from the two
methods can vary widely. In order to avoid any confusion this may cause, turbidity
measurements by the standard nephelometry procedure are now reported in nephelometric
turbidity units (NTU), and the other one is reported in Jackson candle turbidimeter units
(JTU).
40 NTU are about equivalent to 40 JTU.
The applicable range of this method is 0-40 nephelometric turbidity units (NTU). Higher
values may be obtained with dilution of the sample.
Sample handling and preservation:
Water samples should be collected in plastic cans or glass bottles. All bottles must be cleaned
thoroughly and should be rinsed with turbidity free water. Volume collected should be
sufficient to insure a representative sample, allow for replicate analysis (if required), and
minimize waste disposal. No chemical preservation is required. Keep the samples at 4°C.
Do not allow samples to freeze. Analysis should begin as soon as possible after the
collection. If storage is required, samples maintained at 4°C may be held for up to 48 hours.
Precautions:
The following precautions should be observed while performing the experiment:
The presence of coloured solutes causes measured turbidity values to be low.
Precipitation of dissolved constituents (for example, Fe) causes measured turbidity values
to be high.
Light absorbing materials such as activated carbon in significant concentrations can cause
low readings.
The presence of floating debris and coarse sediments which settle out rapidly will give
low readings. Finely divided air bubbles can cause high readings.
Apparatus:
1. Turbidity Meter
Chemicals
1. Formazin Polymer standards
Procedure:
1. For testing the given water sample first the reagents are to be prepared. Then the
turbidity meter is required to be calibrated.
2. To the sample cells, add sample water up to the horizontal mark, wipe gently with soft
tissue and place it in the turbidity meter. Cover the sample cell with the light shield.
3. Check for the reading in the turbidity meter. Wait until you get a stable reading.
19
Assignment
1. Why turbidity is important in “ filtration" and “disinfection" processes?
20
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
21
Experiment 4
Determination of Total Solids, Dissolved Solids
and Suspended Solids in Water
22
Introduction:
Environmental engineering is concerned with the solid material in a wide range of natural
waters and wastewaters. The usual definition of solids (referred to as "total solids") is the
matter that remains as residue upon evaporation at 103~105°C. The various components of
"total solids" can be simplified as follows
Total Solids (TS) are the total of all solids in a water sample. They include the total
suspended solids and total dissolved solids. Total Suspended Solids (TSS) is the amount of
filterable solids in a water sample. Samples are filtered through a glass fiber filter. The filters
are dried and weighed to determine the amount of total suspended solids in mg/l of sample.
Total Dissolved Solids (TDS) are those solids that pass through a filter with a pore size of 2.0
micron (1/1000000th of a meter, Also known as a Micrometer) or smaller. They are said to be
non-filterable. After filtration the filtrate (liquid) is dried and the remaining residue is
weighed and calculated as mg/l of Total Dissolved Solids.
Environmental significance:
Total solids measurements can be useful as an indicator of the effects of runoff from
construction, agricultural practices, logging activities, sewage treatment plant discharges, and
other sources. Total solids also affect water clarity. Higher solids decrease the passage of
light through water, thereby slowing more rapidly and hold more heat; this, in turn, might
adversely affect photosynthesis by aquatic plants. Water will heat up affect aquatic life that
has adapted to a lower temperature regime. As with turbidity, concentrations often increase
sharply during rainfall, especially in developed watersheds. They can also rise sharply during
dry weather if earth-disturbing activities are occurring in or near the stream without erosion
control practices in place. Regular monitoring of total solids can help detect trends that might
indicate increasing erosion in developing watersheds. Total solids are related closely to
stream flow and velocity and should be correlated with these factors. Any change in total
solids over time should be measured at the same site at the same flow. Water with total solids
generally is of inferior palatability and may induce an unfavorable physiological reaction. It
may be esthetically unsatisfactory for purposes such as bathing. Total solids will be higher in
highly mineralized waters, which result in unsuitability for many industrial applications. It
indicates effectiveness of sedimentation process and it affects effectiveness of disinfection
process in killing microorganisms. It is used to assess the suitability of potential supply of
water for various uses. In the case of water softening, amount of total solids determine the
type of softening procedure. Corrosion control is frequently accomplished by the production
of stabilized waters through pH adjustment. The pH stabilization depends to some extent
upon the total solids present as well as alkalinity and temperature.
23
Solids analyses are important in the control of biological and physical wastewater treatment
processes and for assessing compliance with regulatory agency wastewater effluent
limitations
Although the waste water or sewage normally contains 99.9 percent of water and only 0.1
percent of solids, but it is the solids that have the nuisance value. The amount of solids in
wastewater is frequently used to describe the strength of the water. The more solids present in
a particular wastewater, the stronger that wastewater will be. The environmental impacts of
solids in all forms have detrimental effects on quality since they cause putrefaction problems.
If the solids in wastewater are mostly organic, the impact on a treatment plant is greater than
if the solids are mostly inorganic.
In the realm of municipal wastewater, suspended solids analysis is by far the most important
gravimetric method. It is used to evaluate the strength of the raw wastewater as well as the
overall efficiency of treatment. Furthermore, most waste water treatment plants (WWTP’s)
have effluent standards of 10 to 30 mg/L suspended solids which may be legally enforceable.
As was the case with municipal wastewater, suspended solids analysis is useful as a means of
assessing the strength of industrial wastewaters and the efficiency of industrial wastewater
treatment.
Dissolved minerals, gases and organic constituents may produce aesthetically displeasing
color, taste and odor. Some dissolved organic chemicals may deplete the dissolved oxygen in
the receiving waters and some may be inert to biological oxidation, yet others have been
identified as carcinogens. Water with higher solids content often has a laxative and
sometimes the reverse effect upon people whose bodies are not adjusted to them. Estimation
of total dissolved solids is useful to determine whether the water is suitable for drinking
purpose, agriculture and industrial purpose. Suspended material is aesthetically displeasing
and provides adsorption sites for chemical and biological agents. Suspended organic solids
which are degraded anaerobically may release obnoxious odors. Biologically active
suspended solids may include disease causing organisms as well as organisms such as toxic
producing strains of algae. The suspended solids parameter is used to measure the quality of
wastewater influent and effluent. Suspended solids determination is extremely valuable in the
analysis of polluted waters. Suspended solids exclude light, thus reducing the growth of
oxygen producing plants. High concentration of dissolved solids about 3000 mg/L may also
produce distress in livestock. In industries, the use of water with high amount of dissolved
solids may lead to scaling in boilers, corrosion and degraded quality of the product.
24
Guideline:
According to Bangladesh Environment Conservation Rules (1997), potable water should not
contain more than 1000 mg/l of total dissolved solids (TDS).
Principle:
The measurement of solids is by means of the gravimetric procedure. The various forms of
solids are determined by weighing after the appropriate handling procedures. The total solids
concentration of a sample can be found directly by weighing the sample before and after
drying at 103°C. However, the remaining forms, TDS and TSS require filtration of the
sample. For liquid samples, all these solids levels are reported in mg/L.
A rapid assessment of the dissolved solids content of water can be obtained by specific
conductance measurements. Such measurement indicates the capacity of a sample to carry an
electric current which in turn is related to the concentration of ionized substances in the
water. Most dissolved inorganic substances in water are in ionized form and so contribute to
the specific conductance. Although the nature of the various ions, their relative
concentrations, and the ionic strength of the water affect this measurement, such
measurement can give practical estimate of the dissolved mineral content of water. The TDS
content can be approximated by multiplying the specific conductance in micro-Siemens per
cm (µS/cm) by an empirical factor varying from 0.55 to 0.90 depending on the chemical
composition of the TDS.
Sample handling and preservation:
Preservation of sample is not practical. Because biological activity will continue after a
sample has been taken, changes may occur during handling and storage. Both the
characteristics and the amount of solids may change. To reduce this change in samples taken
for solids determinations, keep all samples at 4° C. Do not allow samples to freeze. Analysis
should begin as soon as possible.
Precautions:
The following precautions should be observed while performing the experiment:
Water or Wastewater samples which contain high concentrations of calcium, chloride,
magnesium or sulphate can rapidly absorb moisture from the air. Such samples may
need to be dried for a longer period of time, cooled under proper desiccation and
weighed rapidly in order to achieve a reasonable constant weight. We should be aware
prolonged drying may result in loss of constituents, particularly nitrates and chlorides.
Non-representative particulates such as leaves, sticks, fish and lumps of fecal matter
should be excluded from the sample if it is determined that their inclusion is not
desired in the final result.
Floating oil and grease, if present, should be included in the sample and dispersed by
a blender device before sub-sampling.
Volume of sample should be adjusted to have residue left after drying as 100 to
200mg. It is mainly to prevent large amount of residue in entrapping water during
evaporation.
Highly mineralized water containing significant concentration of calcium,
magnesium, chloride, and/or sulphate may be hygroscopic. Hence prolonged drying,
desiccation and rapid weighing.
We should be aware prolonged drying may result in loss of constituents, particularly
nitrates and chlorides.
25
Apparatus:
1. Balance
2. Beaker
3. Measuring Cylinder
4. Filter paper
5. Funnel
6. Dropper
Procedure:
Measurement of Total Solids (TS)
(1) Take a clear dry glass beaker (which was kept at 103°C in an oven for 1 hour) of 150ml.
capacity and put appropriate identification mark on it. Weight the beaker and note the weight.
(2) Pour 100ml. of the thoroughly mixed sample, measured by the measuring cylinder, in the
beaker.
(3) Place the beaker in an oven maintained at 103°C for 24hours. After 24 hours, cool the
beaker and weight. Find out the weight of solids in the beaker by subtracting the weight of
the clean beaker determined in step (1)
(4) Calculate total solids (TS) as follows:
Calculation:
Total Dissolved Solids, TDS (mg/l) =mg of solids in the beaker x1000 /(volume of sample)
Assignment:
1. Discuss possible sources of solids in ground water and surface water.
2. “Groundwater usually has higher dissolved solids and surface water usually has higher suspended
solids”- Explain.
3. Why water is evaporated at 103°C rather than 100 °C in assessment of solid of water?
26
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
27
Experiment 5
Determination of CO2 in water
28
Introduction:
Carbon Dioxide is present in water in the form of a dissolved gas. Surface waters normally
contain less than 10 ppm free carbon dioxide, while some ground waters may easily exceed
that concentration. Carbon dioxide is readily soluble in water. Over the ordinary temperature
range (0-30°C) the solubility is about 200 times that of oxygen. Calcium and magnesium
combine with carbon dioxide to form carbonates and bicarbonates.
Carbon dioxide does dissolve in water; however the system is somewhat complex. First the
CO2 dissolves according to:
CO2 (g) = CO2 (l) 5.1
3
At room temperature, the solubility of carbon dioxide is about 90 cm of CO2 per 100 ml
water (cl/cg = 0.8). Any water-soluble gas becomes more soluble as the temperature
decreases, due to the thermodynamics of the reaction:
The test for determination of free carbon dioxide in water is based on the titration of water
sample with standard Sodium Hydroxide solution in the presence of phenolphthalein
indicator. The CO2 reacts with NaOH to form Sodium Bicarbonate with a consequent
increase in pH. The reaction of NaOH with free CO2 reach a completion at a pH of 8.3.
Environmental significance:
Aquatic plant life depends upon carbon dioxide and bicarbonates in water for growth.
Microscopic plant life suspended in the water, phytoplankton, as well as large rooted plants,
utilize carbon dioxide in the photosynthesis of plant materials; starches, sugars, oils, proteins.
The carbon in all these materials comes from the carbon dioxide in water.
When the oxygen concentration in waters containing organic matter is reduced, the carbon
dioxide concentration rises. The rise in carbon dioxide makes it more difficult for fish to use
the limited amount of oxygen present. To take on fresh oxygen, fish must first discharge the
carbon dioxide in their blood streams and this is a much slower process when there are high
concentrations of carbon dioxide in the water itself.
29
Corrosion is the principal difficulty caused by carbon dioxide. This gas on solution in water
produces carbonic acid resulting in lowering of pH. With a decrease in pH corrosive
characteristics is induced in water resulting severe corrosion of heat exchanger, pipes, valves
etc. Corrosion in boiler system takes place due to the presence of carbonate and bicarbonate
although Carbon dioxide is not present in this case.
Guidelines:
Bangladesh Environment Conservation Rules (1997) does not set any limits for the presence
of CO2 in water.
Precaution:
Since excess CO2, if present in water, easily escapes to the atmosphere, tests for presence of
CO2 in water should be performed immediately after collection of water sample, especially
for ground water samples which usually contain high CO2. If this is not possible, the sample
bottle should be completely filled and capped and the sample should be kept at a temperature
lower than that at which it was collected.
Where the free CO2 of the water sample is high, there may be some loss of CO2 to the
atmosphere during the titration process. To check this, it is advisable to secure a second
sample. Upon complete determination of CO2 on the first sample, then take the second
sample (100ml) and immediately add the full amount of N/44 sodium hydroxide solution
used in the titration of the first sample. Add 10 drops of phenolphthalein indicator and if the
sample remain colourless, add additional N/44 sodium hydroxide to the end point (till the
slight pink colour appears) and accepting this second test as more accurate titration.
Apparatus:
1. Beaker
2. Measuring cylinder
3. Dropper
4. Stirrer
5. Burette
Reagent:
1. Standard N/44 Sodium Hydroxide
2. Phenolphthalein Indicator **
**An indicator is a substance that undergoes a change in color when the end-point of a
titration is reached. Acid-base indicators are used to signal the end of acid-base titrations. An
acid-base indicator is itself a weak acid (or its conjugate base).
Phenolphthalein is a commonly used indicator for titrations, and is a weak acid. The weak
acid is colorless and its ion is bright pink. Adding extra hydrogen ions shifts the position of
equilibrium to the left, and turns the indicator colorless. Adding hydroxide ions removes the
hydrogen ions from the equilibrium which tips to the right to replace them - turning the
indicator pink. The half-way stage happens at pH 8.3. Since a mixture of pink and colorless is
simply a paler pink, this is difficult to detect with any accuracy.
30
Procedure:
1. Take a 100 ml of sample in a beaker and add 10 drops of Phenolphthalein indicator. If a
pink color develops, no carbon dioxide is present in the water sample.
2. Add N/44 sodium Hydroxide solution from a burette to the sample and stir gently until a
slight permanent pink color appears as compared with distilled water. Record ml of
sodium hydroxide used. Since excess CO2, if present easily escapes to atmosphere, so
tests should be performed immediately after collection of water sample. If this is not
possible sample bottle should be completely filled and stoppered and be kept at a
temperature lower than that at which it was collected.
Calculation:
Carbon dioxide (mg/L) =mL of N/44 NaOH used x Multiplying Factor (M.F.)
Where, M.F. =
Hence, Acidity could be easily determined from the results of CO2 determination as follows:
Assignment:
1. Discuss changes in the form of Carbon in solution at different pH.
2. Why does groundwater contain higher carbon dioxide then surface water?
3. Why test for Carbon dioxide should be performed immediately after collection of water sample?
31
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
Burette Reading
Volume (mL)
Sample No Temperature Volume of CO2
of CO2 acidity
and of Sample NaOH Concentration
Sample (mg/L as CaCO3)
source (°C) Initial Final (mL) (mg/L)
(mL)
32
Experiment 6
Determination of Alkalinity in Water
33
Introduction:
Alkalinity is primarily a way of measuring the acid neutralizing capacity of water. In other
words, its ability to maintain a relatively constant pH. The possibility to maintain constant pH
is due to the hydroxyl, carbonate and bicarbonate ions present in water. The ability of natural
water to act as a buffer is controlled in part by the amount of calcium and carbonate ions in
solution.
Carbonate ion and calcium ion both come from calcium carbonate or limestone. So water that
comes in contact with limestone will contain high levels of both Ca++ and CO32- ions and
have elevated hardness and alkalinity.
Environmental significance:
Alkalinity is important for fish and aquatic life because it protects or buffers against rapid pH
changes. Higher alkalinity levels in surface waters will buffer acid rain and other acid wastes
and prevent pH changes that are harmful to aquatic life. Large amount of alkalinity imparts
bitter taste in water. The principal objection of alkaline water is the reactions that can occur
between alkalinity and certain actions in waters. The resultant precipitate can corrode pipes
and other accessories of water distribution systems.
Wastewaters containing excess caustic (hydroxide) alkalinity are not to be discharged into
natural water bodies or sewers. Alkalinity as carbonate and bicarbonate of saline water is
very important in tertiary recovery processes for recovering petroleum. Alkaline water offers
better wetting to the formation rock and improve oil release. As an additional benefit, ions
that provide alkalinity absorb on rock surfaces occupying adsorption sites and decrease the
loss of recovery chemical by adsorption. The alkalinity value is necessary in the calculation
of carbonate scaling tendencies of saline waters.
Principle:
The alkalinity of water can be determined by titrating the water sample with sulphuric acid of
known values of pH, volume and concentrations. Based on stoichiometry of the reaction and
number of moles of sulphuric acid needed to reach the end point, the concentration of
alkalinity in water is calculated. When a water sample that has a pH of greater than 4.5 is
titrated with acid to a pH 4.5 end point, all OH-, CO32-, and HCO3- will be neutralized.
For the pH more than 8.3, add phenolphthalein indicator, the colour changes to pink colour.
This pink colour is due to presence of hydroxyl ions. If sulphuric acid is added to it, the pink
colour disappears i.e. OH- ions are neutralized. Then add methyl orange indicator, the
presence of CO32- and HCO3- ions in the solution changes the colour to yellow. While adding
sulphuric acid, the color changes to slight orange ting, this color change indicates that all the
CO32- and HCO3- ions has been neutralized. This is the end point.
34
Apparatus:
1. Burette with Burette stand and porcelain title
2. Pipettes with elongated tips
3. Conical flask
4. Measuring cylinders
5. Beakers
6. Dropper
7. Stirrer
Chemicals
1. Standard0.02N sulphuric acid
2. Phenolphthalein indicator
3. Methyl orange indicator
Sample handling and preservation:
Preservation of sample is not practical. Because biological activity will continue after a
sample has been taken, changes may occur during handling and storage. To reduce the
change in samples, keep all samples at 4°C. Do not allow samples to freeze. Analysis should
begin as soon as possible. Do not open sample bottle before analysis.
Procedure:
1. Measure 50 ml or 100 ml of your sample into a 250 mL beaker or erlenmyer flask. Place
your sample onto a stir plate (make sure to put a bar magnet in the flask).
2. Measure initial pH of your sample. If the sample pH is below 8.3 (if above 8.3, do step 3
first), add several drops of methyl orange indicator. If the color of the solution turned
yellow, titrate your sample with 0.02 N H2SO4 (you may need to dilute the acid provided
in the lab) until the color changes to slightly orange ting (pH 4.5). Record the total
volume of acid used for the titration.
3. Measure initial pH of your sample. If the sample pH is above 8.3, add several drops of
phenolphthalein indicator. If the color of the solution turned pink, titrate your sample with
0.02 N H2SO4 or HCl (you may need to dilute the acid provided in the lab) until color
changes from pink to clear (pH 8.3). Record the volume of acid used for the titration.
Then, proceed with step 2.
4. Calculate both Phenolphthalein Alkalinity and Total Alkalinity using the formula
provided above.
Calculation:
Phenolphthalein Alkalinity (mg/L as CaCO3)
= Multiplying Factor (MF) x milliliter of 0.02N H2SO4(added up to pH 8.3)
Total Alkalinity (mg/L as CaCO3)
=Multiplying Factor (MF) x milliliter of 0.02N H2SO4(added up to pH approx. 4.5)
Where, M.F. =
Assignment:
1. Discuss the importance of alkalinity in water for different treatment processes.
2. Define total alkalinity, phenolphthalein alkalinity, and methyl orange alkalinity. Discuss their
dominant pH range.
35
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
36
Experiment 7
Determination of Hardness in Water
37
Introduction:
Hard waters are generally considered to be those waters that require considerable amounts of
soap to produce foam or leather and that also produce scale in hot-water pipes, boilers, and
other units in which the temperature of water is increased substantially. The hardness of
water varies considerably from place to place. In general, surface water is softer than
groundwater. The hardness of water reflects the nature of the geological formations with
which it has been in contact.
Hardness is caused by multivalent metallic cations. Such cations are capable of reacting with
soap to form precipitates and with certain anions present in water to form scale. The principal
hardness causing cations are the divalent calcium, magnesium, strontium, ferrous ion and
manganaous ions. These cations and the important anions with they are associated with are
shown in the following table in the order of their relative abundance in natural waters.
Aluminum and ferric ions are sometimes considered as contributing to the hardness of water.
However, their solubility is so limited at pH values of natural waters that ionic concentrations
are negligible. The hardness of water is derived largely from contact with the soil and rock
formations.
Table-7.1: Principal hardness causing cations and the major anions associated with them
Where, M2+ = concentration of divalent metal cation (mg/l) and 50 is the equivalent weight of
CaCO3.
=∑[ ] 7.3
Environmental significance:
Hard water is as satisfactory for human consumption as soft waters. Because of their action
with soap, however, their use for cleansing purpose is quite unsatisfactory, unless soap costs
are disregarded. Soap consumption by hard waters represents an economic loss to the water
user. Sodium soaps react with multivalent metallic cations to form a precipitate, thereby
losing their surfactant properties. In recent years these problems have been largely alleviated
by the developments of soaps and detergents that do not react with hardness.
Boiler scale, the result of the carbonate hardness precipitation, may cause considerable
economic loss through fouling of water heater and hot water pipes. Change in pH in the water
38
distribution systems may also result in deposits of precipitates. Bicarbonates begin to convert
to the less soluble carbonates at pH values above 9.0.
Magnesium hardness, particularly associated with the sulfate ion has a laxative effect on
persons unaccustomed to it. Magnesium concentrations of less than 50 mg/l are desirable in
potable waters, although many public water supplies exceed the amount. Calcium hardness
presents no public health problem. In fact, hard water is apparently beneficial to the human
cardiovascular system. Water can be generally classified in terms of the degree of hardness as
follows:
Table 7.2: Water quality with respect to hardness
Hardness
Water Quality
(mg/l as CaCO3)
Soft <50
Moderately hard 50-150
Hard 150-300
Very hard >300
39
Reagents:
1. Buffer solution (for attaining a pH close to 10.0)
2. Erichrome Black T dye
3. Standard EDTA solution
Apparatus:
1. Beaker
2. Measuring cylinder
3. Dropper
4. Stirrer
5. Auto-titration device
Procedure:
1. Take 50 ml sample in a 150 ml beaker.
2. Add one ml of standard buffer solution (supplied by HACH) to raise the pH of water
sample to about 10.0.
3. Add one packet of Erichome Black T dye(supplied by HACH) indicator to the beaker.
The sample would turn wine red (if hardness is present).
4. Fit the cartridge containing standard EDTA solution to the titrator device (supplied by
HACH).
5. Turn the flow control knob of the device until the solution starts to come out of the
tube fitted to the cartridge. Take initial reading of the counter.
6. Immerse the tube fitted to the cartridge into the water sample and start titrating (under
constant stirring) by turning the flow control knob of the auto-titrator. Continue until
the wine red colour of the sample changes to blue. Take final reading of the counter.
Calculation:
Total hardness (mg/L as CaCO3)
= Multiplying Factor (MF) x (initial counter reading – final counter reading)
Where, M.F. =
40
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
Burette Reading
Volume (mL) Volume of
Sample No Temperature Hardness
of EDTA
and of Sample Concentration
Sample solution
source (°C) Initial Final (mg/L as CaCO3)
(mL) (mL)
41
Experiment 8
Determination of Chloride in water
42
Introduction:
Chlorides occur in all natural waters in widely varying concentration, the chloride content
normally increases as the mineral content increases. Upland and mountain supplies usually
are quite low in chlorides, whereas river and groundwater usually have a considerable
amount. Sea and ocean waters represent the residues resulting from partial evaporation of
natural waters that flow into them and chloride levels are very high. Chlorides gain access to
natural waters in many ways. The solvent power of water dissolves chlorides from topsoil
and deeper formations. Spray from the ocean is carried inland as droplets or as minute salt
crystals, which result from evaporation of the water in the droplets. These sources constantly
replenish the chlorides in inland areas where they fall. Ocean and seawaters invade the rivers
that drain into them, particularly the deeper rivers. The salt water, being denser, flows
upstream under the fresh water, which is flowing downstream. There is a constant
intermixing of the salt water with the fresh water above. Groundwater in areas adjacent to the
ocean is in hydrostatic balance with seawater. Over-pumping of groundwater produces a
difference in hydrostatic head in favor of the seawater, and it introduce into the fresh water
area. Such intrusion has occurred in many areas of the coastal southern region of Bangladesh.
Human excreta, particularly urine, contain chloride in an amount about equal to the chlorides
consumed with food and water. This amount average about 6 gm of chlorides per person per
day and increases the amount of CC in municipal wastewater about 15 mg/l above that of the
carriage water. Thus, wastewater effluents add considerable chlorides to receiving streams.
Many industrial wastes (e.g., tannery waste) also contain appreciable amount of chlorides.
Environmental significance:
Chlorides in reasonable concentrations are not harmful to human. At concentrations above
250 mg/L they give a salty taste to water, which is objectionable to many people. For this
reason, chlorides are generally limited to 250 mg/L in supplies intended for public use. In
many areas of the world where water supplies are scarce, source be containing as much as
2,000 mg/L are used for domestic purposes without the development of adverse effects, once
the human system becomes adapted to the water.
Guideline:
According to Bangladesh Environment Conservation Rules (1997), drinking water standard
for chloride is 150 - 600 mg/L; but for coastal regions of Bangladesh, the limit has been
relaxed to 1000 mg/L.
The end point of the titration occurs when all the chloride ions are precipitated. Then
additional silver ions react with the chromate ions of the indicator, potassium chromate, to
form a red-brown precipitate of silver chromate.
2Ag+(aq) + CrO42–(aq)→ Ag2CrO4(s) 8.2
This method can be used to determine the chloride ion concentration of water samples from
many sources such as seawater, stream water, river water and estuary water. The pH of the
sample solutions should be between 6.5 and 10. If the solutions are acidic, the gravimetric
method or Volhard’s method should be used.
43
***The end point of titration cannot be detected visually unless an indicator capable of
demonstrating the presence of excess Ag+ is present. The indicator normally used is
potassium chromate, which supplies chromate ions. As the concentration of CI- ions becomes
exhausted, the silver ion concentration increases and a reddish brown precipitate of silver
chromate is formed.
2Ag++CrO42- = Ag2CrO4 (reddish brown precipitate) 8.3
This is taken as evidence that all chloride has been precipitated. Since an excess Ag+ is
needed to produce a visible amount of Ag2CrO4, the indicator error is subtracted from all
titrations.
The indicator error or blank varies somewhat with the ability of individuals to detect a
noticeable color change. The usual range is 0.2 to 0.4 mL of titrant. An error of 0.2 mL will
be used in the class.
Precautions:
1. A uniform sample size must be used, preferably 100 ml (or 50 mL), so that ionic
concentrations needed to indicate the end point will be constant.
2. The pH must be in the range of 7 to 8 because Ag+ is precipitated as AgOH at high pH
levels and the CrO42- is converted to Cr2O72- at low pH levels,
3. A definite amount of indicator must be used to provide a certain concentration of CrO4;
otherwise Ag2CrO4 may form too soon or not soon enough.
4. The chromate solution needs to be prepared and used with care as chromate is a known
carcinogen.
5. Silver nitrate solution causes staining of skin and fabric (chemical burns). Any spills
should be rinsed with water immediately.
Apparatus:
1. Burette
2. Measuring cylinder
3. Beaker
4. Dropper
5. Stirrer
Reagents:
1. Potassium chromate indicator
2. Silver nitrate solution (0.0141 N)
Procedure:
1. Take 50 mL of the sample in a beaker and add 5 drops (about 1 mL) of potassium
chromate indicator to it.
2. Add standard (0.0141 N) silver nitrate solution to the sample from a burette, a few
drops at a time, with constant stirring until the first permanent reddish color appears.
This can be determined by comparison with distilled water blank. Record the mL of
silver nitrate used.
3. If more than 7 or 8 mL of silver nitrate solution are required, the entire procedure should
be repeated using a smaller sample diluted to 50 ml with distilled water.
44
Calculation:
Where, M.F. =
Assignment
1. "Chlorides can introduce into natural waters in many ways" --explain.
2. Why it is necessary to dilute sample if end point does not obtained even after adding more than 7
or 8 mL silver nitrate to the original sample?
3. In determination of chloride, why an indicator "blank" or "error" is subtracted from the amount of
silver nitrate used in titration? Explain.
45
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
Burette Reading
Volume (mL) Volume of
Sample No Temperature Chloride
of AgNO3
and of Sample Concentration
Sample solution
source (°C) Initial Final (mg/L)
(mL) (mL)
46
Experiment 9
Determination of Total Iron in Water
47
Introduction:
Iron, as well as manganese, creates serious problems in public water supplies. The
problems are most critical for groundwater. Iron exists in soils and minerals as insoluble
ferric oxide/hydroxide and iron sulphide (pyrite). In some areas, it also occurs as ferrous
carbonate, which is very slightly soluble. Since groundwater usually contains significant
amounts of carbon dioxide, appreciable amounts of ferrous carbonate may be dissolved
according to Eq.9.1.
Environmental significance:
As far as is known, human suffer no harmful effects from drinking waters containing iron
and manganese. Such waters, when exposed to the air so that oxygen can enter,
become turbid and highly unacceptable from the aesthetic' viewpoint owing to the
oxidation of iron and manganese to the Fe3+, and Mn4+ states which form colloidal
precipitates. The rates of oxidation are not rapid, and thus reduced forms can persist for
some time in aerated waters. This is especially true when the pH is below 6 with iron
oxidation and below 9 with manganese oxidation. The rates may be increased by the
presence of certain inorganic catalysts through the action of microorganisms.
Both iron and manganese interfere with laundering operations, impart objectionable
stains to plumbing fixtures and cause difficulties in distribution systems by supporting
growths of iron bacteria. Iron also imparts a taste to water, which is detectable at very
low concentrations.
Guideline:
According to Bangladesh Environment Conservation Rules (1997), drinking water standard for
iron is 0.3 - 1.0 mg/l.
The quantity of ferric iron is determined by comparison with the red color produced by
standard iron solutions.
Apparatus:
1. Nessler tube
2. Measuring cylinder
3. Dropper
Reagents:
1. Hydrochloric acid
2. Potassium permanganate solution
3. Potassium thiocyanate solution
4. Standard iron solution
Procedure:
1. Place 100 mL of the water sample in a Nessler.
2. Add 5 mL of dilute hydrochloric acid
3. Add two drops of potassium permanganate solution
4. Add 5 mL of potassium thiocyanate solution. The solution would turn brown if iron
is present.
5. Compare the brown color formed with the standard prepared as follows:
a.Add 100 mL of distilled water in a Nessler tube
b.Add 5 mL of the dilute hydrochloric acid.
c.Add two drops of potassium permanganate solution.
d.Add 5 mL of potassium thiocyanate solution.
e.Add 0.2 mL at a time of the standard iron solution until the color of the standard
and the sample match.
Calculation:
Standard iron solution added in distilled water(mL) x Conc. of standard iron solution(mg/L)
mL of sample taken
49
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
50
Experiment 10
Determination of Arsenic in Water
51
Introduction:
Presence of elevated levels of arsenic in groundwater (especially from shallow aquifer) has
become a major concern in Bangladesh. Arsenic pollution of groundwater is particularly
challenging in Bangladesh since tubewell water extracted from shallow aquifers is the major
source of drinking water for most of its population. The rural water supply is almost entirely
based on groundwater supply through use of hand pump tubewells; the urban water' supply is
also heavily dependent on groundwater. In Bangladesh, the arsenic in groundwater is of
geologic origin and is probably only apparent now because it is only the last 20 - 30 years
that groundwater has been extensively used for drinking in rural areas.
Weathering of arsenic-rich base metal sulphides in the upstream of the Ganges basin appears
to be a major source of arsenic-rich iron oxyhydroxides in the sediments of Bangladesh. Use
of phosphate fertilizer can potentially enhance release of arsenic as a result of replacement of
arsenic by phosphate ions on the adsorption sites of iron oxyhydroxides. Natural and
anthropogenic processes that may lead to release/mobilization of arsenic in the subsurface are
being investigated.
Arsenic occurs in water in several different forms. Depending upon the pH and the redox
potential, Eh. Some of the most important compounds and species are shown in Table 1.
Table 1: Arsenic compounds and species and their environmental and toxicological
importance in water
Guideline:
According to ECR 1997, drinking water standard for arsenic in Bangladesh is 50 μg/L(or
0.05 mg/L). The WHO guideline value for arsenic in drinking water is 10μg/Land the
USEPA is also planning to revise its standard from50 μg/Lto10μg/L.
Apparatus:
1. Arsenic toolkits
Procedure:
1. Add reagent to Reaction Bottle and shake vigorously.
2. Insert the strip into the turret and close it. Let it sit 10 minutes.
3. Select the As concentration on the chart that matched the color of the test strip most
closely. The reference chart provided with the kit displays the yellow to brown range of
colors expected for As concentrations of 0, 10, 25, 50, 100, 200, 300, 500, and 1000 μg/L.
Assignment:
1. Discuss possible sources of arsenic in ground water.
2. Does the toxicity of arsenic contaminated groundwater depend on arsenic speciation?
54
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
55
Experiment 11
Determination of Biochemical oxygen demand
56
Introduction:
The biochemical oxygen demand determination is a chemical procedure for determining the
amount of dissolved oxygen needed by aerobic organisms in a water body to break the
organic materials present in the given water sample at certain temperature over a specific
period of time.
BOD of water or polluted water is the amount of oxygen required for the biological
decomposition of dissolved organic matter to occur under standard condition at a
standardized time and temperature. Usually, the time is taken as 5 days and the temperature is
20°C.
The test measures the molecular oxygen utilized during a specified incubation period for the
biochemical degradation of organic material (carbonaceous demand) and the oxygen used to
oxidize inorganic material such as sulfides and ferrous ion. It also may measure the amount
of oxygen used to oxidize reduced forms of nitrogen (nitrogenous demand).
Environmental significance:
BOD is the principle test to give an idea of the biodegradability of any sample and strength of
the waste. Hence the amount of pollution can be easily measured by it. Efficiency of any
treatment plant can be judged by considering influent BOD and the effluent BOD and so also
the organic loading on the unit.
Application of the test to organic waste discharges allows calculation of the effect of the
discharges on the oxygen resources of the receiving water. Data from BOD tests are used for
the development of engineering criteria for the design of wastewater treatment plants.
Ordinary domestic sewage may have a BOD of 200 mg/L. Any effluent to be discharged into
natural bodies of water should have BOD less than 30 mg/L. This is important parameter to
assess the pollution of surface waters and ground waters where contamination occurred due
to disposal of domestic and industrial effluents. Drinking water usually has a BOD of less
than 1 mg/L. But, when BOD value reaches 5 mg/L, the water is doubtful in purity. The
determination of BOD is used in studies to measure the self-purification capacity of streams
and serves regulatory authorities as a means of checking on the quality of effluents
discharged to stream waters.
The determination of the BOD of wastes is useful in the design of treatment facilities. It is the
only parameter, to give an idea of the biodegradability of any sample and self-purification
capacity of rivers and streams. The BOD test is among the most important method in sanitary
analysis to determine the polluting power, or strength of sewage, industrial wastes or polluted
water. It serves as a measure of the amount of clean diluting water required for the successful
disposal of sewage by dilution.
Guideline:
According to Bangladesh Environment Conservation Rules (1997), drinking water standard
for biochemical oxygen demand (BOD) is 0.2 mg/L (at 20°C). For wastewater effluent
allowable concentration of BOD varies from 50- 250 mg/L depending on discharge point of
the effluent (e.g., inland water, irrigation land, public sewer etc.)
Principle:
The sample is filled in an airtight bottle and incubated at specific temperature for 5 days. The
dissolved oxygen (DO) content of the sample is determined before and after five days of
incubation at 20°C and the BOD is calculated from the difference between initial and final
DO. The initial DO is determined shortly after the dilution is made; all oxygen uptake
occurring after this measurement is included in the BOD measurement.
57
Since the oxygen demand of typical waste is sever hundred milligrams per liter, and since the
saturated value of DO for water at 20uC is only 9.1 mg/L, it is usually necessary to dilute the
sample to keep final DO above zero. If during the five days of experiment, the DO drops to
zero, then the test is invalid since more oxygen would have been removed had more been
available.
Here,
Dilution factor (D.F.) =
In some cases, it becomes necessary to seed the dilution water with microorganisms to ensure
that there is an adequate bacterial population to carry out the biodegradation. In such cases,
two sets of BOD bottles must be prepared, one for just the seeded dilution water (called the
"blank") and the other for the mixture of wastewater and dilution wader. The changes in DO
in both are measured. The oxygen demand of waste water (BODw) is then determined from
the following relationship:
Where, BODm, is the BOD of the mixture of wastewater and dilution water and BODd is the
BOD of the dilution water alone; Vw and Vd are the volumes of wastewater and dilution water
respectively in the mixture and Vm = Vw + Vd.
58
Procedure:
Fill two BOD bottles with sample (or diluted sample); the bottles should be completely filled.
Determine initial DO (DOi) in one bottle immediately after filling with sample (or diluted
sample). Keep the other bottle in dark at 20°C and after particular days (usually 5-days)
determine DO (DOf) in the sample (or diluted sample). Dissolved oxygen (DO) is determined
according to the following procedure:
1. Add 1 mL of manganous sulfate solution to the BOD bottle by means of pipette,
dipping in end of the pipette just below the surface of the water.
2. Add 1 mL of alkaline potassium iodide solution to the BOD bottle in a similar
manner.
3. Insert the stopper and mix by inverting the bottle several times.
4. Allow the "precipitates" to settle halfway and mix again.
5. Again allow the "precipitates" to settle halfway.
6. Add 1 mL of concentrated sulfuric acid. Immediately insert the stopper and
mix as before.
7. Allow the solution to stand at least 5 minutes.
8. Withdraw 100 mL of solution into an Erlenmeyer flask and immediately add 0.025N
sodium thiosulfate drop by drop from a burette until the yellow color almost
disappears.
9. Add about 1 mL of starch solution and continue the addition of the thiosulfate
solution until the blue color just disappears. Record the ml. of thiosulfate solution
used (disregard any return of the blue color).
Calculation:
Assignment:
1. In a BOD test on a diluted wastewater sample (1:20 dilution, but not seeded), the initial DO is 8.2
mg/L and final DO after 5 days is 3.2 mg/L. If the reaction rate constant is 0,2/day, calculate: (a)
5-day BOD of the wastewater, (b) Ultimate carbonaceous BOD of the wastewater, (c) Remaining
Oxygen demand after 5-days.
2. A test bottle containing just seeded dilution water has its DO level drop by 0.6 mg/L in a 5-day
test, A 300 mL BOD bottle filled with 40 mL of wastewater and the rest with seeded dilution
water experiences a drop of 7.1 mg/L in the same period (5-day), Calculate the BOD5 of the
wastewater.
59
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
60
Experiment 12
Determination of Chemical oxygen demand
61
Introduction:
The chemical oxygen demand (COD) test allows measurement of oxygen demand of the
waste in terms of the total quantity of oxygen required for oxidation of the waste to carbon
dioxide and water. The test is based on the fact that all organic compounds, with a few
exceptions, can be oxidized by the action of strong oxidizing agents under acid conditions.
The reaction in Eq.-1 involves conversion of organic matter to carbon dioxide and water
regardless of the biological assimilability of the substance. For example, glucose and lignin
(biologically inert substance) are both oxidized completely by the chemical oxidant. As a
result, COD values are greater than BOD values, especially when biologically resistant
organic matter is present.
Thus one of the chief limitations of COD test is its inability to differentiate between
biodegradable and non-biodegradable organic matter. In addition, it does not provide any
evidence of the rate at which the biologically active material would be stabilized under
conditions that exist in nature.
The major advantage of COD test is the short time required for evaluation. The determination
can be made in about 3 hours rather than the 5-days required for the measurement of BOO.
For this reason, it is used as a substitute for the BOD test in many instances.
Environmental Significance:
"COD is often measured as a rapid indicator of organic pollutant in water; it is normally
measured in both municipal and industrial wastewater treatment plants and gives an
indication of the efficiency of the treatment process. COD has further applications in power
plant operations, chemical manufacturing, commercial laundries, pulp & paper mills,
environmental studies and general education.
Guideline:
According to Bangladesh Environment Conservation Rules (1997), drinking water standard
for chemical oxygen demand (COD) is 4.0 mg/L. For wastewater effluent allowable
concentration of CBOD varies from 200- 400 mg/L depending on discharge point of the
effluent (e.g., inland water, irrigation land, public sewer etc.)
Principle:
Potassium dichromate or potassium permanganate is usually used as the oxidizing agent in
the determination of COD. In this class potassium permanganate would be used in the
determination of COD. Potassium permanganate is selective in the reaction and attacks the
carbonaceous and not the nitrogenous matter.
In any method of measuring COD, an excess of oxidizing agent must be present to ensure
that all organic matter is oxidized as completely as possible within the power of the reagent.
This requires that a reasonable excess be present in all samples. It is necessary, therefore, to
measure the excess in some manner so that the actual amount can be determined. For this
purpose, a solution of a reducing agent (e.g., ammonium oxalate) is usually used.
Apparatus:
1. Beaker (250 mL)
2. Dropper
3. Stirrer
62
Reagent:
1. Diluted sulfuric acid solution
2. Standard potassium permanganate solution
3. Standard Ammonium Oxalate solution
Procedure:
1. Pipette 100 mL of the sample into a 250 mL Erlenmeyer flask.
2. Add 10 mL of diluted sulfuric acid and 10 mL of standard KMn04 solution.
3. Heat the flask in a boiling water bath for exactly 30 minutes, keeping the water in the bath
above the level of the solution in the flask. The heating enhances the rate of oxidation
reaction in the flask.
4. If the solution becomes faintly colored, it means that most of the potassium permanganate
has been utilized in the oxidation of organic matter. In such a case, repeat the above using
a smaller sample diluted to 100 mL with distilled water.
5. After 30 minutes in the water bath, add 10 mL of standard ammonium oxalate
[(NH4)2C204] solution into the flask. This 10 mL ammonium oxalate, which is a reducing
agent, is just equivalent to the 10 mL potassium permanganate (oxidizing agent) added
earlier. The excess of reducing agent [(NH4)2C204] now remaining in the flask is just
equivalent to the amount of the oxidizing agent (KMn04) used in the oxidation of organic
matter.
6. The quantity of ammonium oxalate remaining in the flask is now determined by titration
with standard potassium permanganate. Titrate the content of the flask while hot with
standard potassium permanganate to the first pink coloration. Record the mL of
potassium permanganate used.
Calculation:
COD (mg/L) =
Assignment:
1. What are the principal advantages and disadvantages of the COD test over the BOD test?
2. Explain why COD values are greater than BOD values.
63
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
64
Experiment 13
Chemical Coagulation of water:
Alum Coagulation
65
Introduction:
Chemical coagulation is a treatment method widely used for removal of small sized and
colloidal impurities from water. Surface water generally contains a wide variety of colloidal
impurities that may cause the water to appear turbid and may impart color to the water.
Colloidal particles that cause color and turbidity are difficult to separate from water because
the particles will not settle by gravity and are so small that they pass through the pores of
most common filtration media. In order to be removed, the individual colloids must aggregate
and grow in size so that they can settle by gravity. Chemical agents are used to promote
colloid aggregation by destroying the forces that stabilize colloidal particles.
The process of destroying the stabilizing forces and causing aggregation of colloids is
referred to as chemical coagulation. Coagulation involves reduction of electrical forces of
repulsion and promotion of "chemical type" interaction between colloids, which eventually
results in settling of the colloids and accomplishes removal of turbidity and color. At higher
coagulant doses, "charge reversal" is possible which may result in re-suspension of the
colloids. Hence optimum coagulant doses are determined through laboratory model tests
where the water to be treated are subjected to a range of doses of a coagulant and the removal
efficiencies are observed.
Many authors use the term "coagulation" to describe the process by which the charge on
particles is destroyed, and the term "flocculation" to describe the aggregation of particles into
larger units. The chemical used for this purpose is called are called coagulants. The most
common coagulants used in water and wastewater treatment are aluminum and ferric salts
such as alum, ferric chloride and ferric sulfate.
The common metal salt alum (aluminum sulfate) is a good coagulant for water containing
appreciable organic matter. The chemical formula used for commercial alum is
Al2(SO4)3.14H20. Once dissolved in water, aluminum forms hydroxo-complexes and solids
[e.g., Al(OH)3(s), Al(OH)2+, Al(OH)2+, Al(OH)4-; and as a result pH of water is lowered,
especially if alkalinity of water is low,. Theoretically, each mg/L of alum consume
approximately 0.50 mg/L (as CaCO3) of alkalinity, For water with low alkalinity, this may
result in significant reduction in pH that may interfere with formation of aluminum hydroxide
flocs. If the alkalinity is insufficient, coagulant aids such as lime [Ca(OH)2], soda ash
(Na2CO3), activated silica and polyelectrolytes are used to provide the necessary alkalinity.
Iron coagulants can be operated over a wider pH range and are generally effective in
removing turbidity and color from water. However, they are usually more costly.
Environmental Significance:
Besides efficient removal of turbidity and color, coagulation with alum and ferric chloride or
ferric sulfate is also widely used for removal of heavy metal ions (e.g., lead, arsenic) from
water. In this process heavy metal ions are primarily removed by adsorption (and Subsequent
precipitation) onto coagulated flocs of metal (either aluminum or iron) hydroxides.
Coagulation with alum and ferric chloride / sulfate is being successfully used for removal of
arsenic from water.
66
Principle:
Treatment of water by coagulation involves -
(1) Determination of optimum dose of coagulant by jar test.
(2) Determination of power input for the flocculator.
In the class jar test to determine optimum coagulant dose will be carried out, it is important to
determine the optimum dose to avoid charge reversal and resuspension colloids. Optimum
coagulant dose is considered as the amount of coagulant which produces water with lowest
turbidity.
Apparatus:
1. Coagulation (stirring) device
2. pH meter
3. Turbidity meter
4. Glass beakers (1000 mL)
Reagent:
1. Standard Alum solution.
Procedure:
1. Determine pH and turbidity of the water to be treated. You may be instructed to
determine color and arsenic concentration of the water to be treated (if removal
efficiencies of these parameters are to be determined).
2. Fill six 1000 mL beakers each with 500 mL water to be treated,
3. Add required (as instructed by teacher) coagulant (standard alum solution) to each beaker.
4. Mix the samples in the beaker with the help of the stirring device. Subject the samples to
one minute of rapid mixing followed by 15 minutes of slow mixing (about 40 rpm).
5. Allow the flocs to settle down for about 15 minutes. Observe the characteristics of the
flocs and the settling rates.
6. Collect the supernatant from each beaker and measure pH and turbidity of each. You may
be instructed to measure color and arsenic concentration of the supernatant samples (if
removal efficiencies of these parameters are to be determined).
7. Plot pH versus alum dose in a graph paper and observe effect of alum dose on pH.
8. Plot turbidity (NTU) versus the coagulant (alum) dose (mg/L) in a graph paper.
Determine optimum dose of alum from this plot.
Assignment:
1. What is charge reversal? When and why it happens?
2. Why addition of alum may result in a drop in pH value. Discuss the effect of alum dose on pH
from your experimental results.
67
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
Initial
Observation Alum Dose Final
pH (initial) Turbidity pH (final)
No. (mg/L) Turbidity
(NTU) (NTU)
68
Experiment 14
Break Point Chlorination
69
Introduction:
Chlorination of public water supplies and polluted waters serves primarily to destroy or de-
activate disease-producing microorganisms. Disinfection with chlorine is widely practiced.
Chlorination may produce some adverse effects including taste and odor problem. in recent
years, chlorination has been found to produce trihalomethanes (THMs) and other organics of
health concern (THMs are suspected human carcinogens). Thus, use of alternative
disinfectants, such as chlorine dioxide and ozone that do not cause this particular problem, is
increasing.
Theory:
Disinfectant capabilities of chlorine depend on its chemical form in water, which in turn is
dependent on pH, temperature, organic content of water, and other water quality factors.
Chlorine is used in the form of free chlorine [e.g., chlorine gas] or as hypochlorites [e.g.,
NaOCl and Ca(OC1)2]. Chlorine applied to water either as free chlorine or hypochlorite
initially undergoes hydrolysis to form free chlorine consisting of aqueous molecular chlorine,
hypochlorous acid and hypochlorite ion.
The two chemical species formed by chlorine in water, hypochlorous acid (HOCl) and
hypochlorite ion (OCl–), are commonly referred to as “free” or “available” chlorine.
70
Figure 13.1 shows that Cl2 can be significantly at low pH values (below pH 2); while HOCl is
dominant between pH 3 and 6. Between pH 6 and 9, the relative fraction of HOCl decrease,
while the corresponding fraction of OCl- increases. In waters with pH between 6.5~8.5, the
reaction is incomplete and both species (HOCl and OCl-) will be present. Hypochlorous acid
is the more germicidal of the two, especially at short contact time. The dissociation of HOCl
is also temperature dependent. The effect of temperature is such that at a given pH, the
fraction of HOCl will be lower at higher temperatures.
The mono- and dichloramines have significant disinfecting power and are therefore of
interest in the measurement of chlorine residuals. Combined chlorine in water supplies may
be formed in the treatment of raw waters containing ammonia; chlorinated wastewater
effluents, as well as certain chlorinated industrial effluents normally contain only combined
chlorine.
72
Environmental Significance:
Breakpoint chlorination is required to obtain a free chlorine residual for better disinfection if
ammonia is present in a water supply. While free chlorine residuals have good disinfecting
powers, they are usually dissipated quickly in the distribution system. For this reason, final
treatment with ammonia if often practiced to convert free chlorine residuals to longer-lasting
combined chlorine residuals. The difference between the amount of chlorine added to the
water and the amount of residual chlorine (i.e., free and combined available chlorine
remaining) at the end of a specified contact period is termed as "chlorine demand'.
Apparatus:
1. Erlemeyer flask (250 mL)
2. Bottle
3. Beaker (250 mL)
4. Measuring cylinder
5. Dropper
6. Stirrer
Reagents:
1. Starch Indicator
2. Standard 0.025 N Sodium thiosulfate
3. Potassium Iodine crystal
4. Concentrated Acetic Acid
5. Chlorine water
Procedure:
1. Place 200-mL portion of the water to be chlorinated in each of six 250-mL flasks.
2. Add required quantity (as instructed by your teacher) of "chlorine water" (stock solution
of bleaching powder in water) in each of the flasks. The chlorine content of the "chlorine
water" (determined earlier in the laboratory) would be provided to you by your teacher.
Calculate the chlorine dose for each of the six flasks.
3. Shake each flask gently and allow to stand for 30 minutes.
4. Determine residual chlorine of water from each flask by the starch-iodine method as
described below:
Starch-Iodine Method:
The starch-iodine method is based on the oxidizing power of free and combined chlorine
residuals to convert iodide ion into free iodine at pH 8 or less, as shown below.
Cl2 + 2I- = I2 + 2 Cl-
In the starch-iodine method, the quantity of chlorine residuals is determined by measuring the
quantity of iodine by titration with a reducing agent sodium thiosulfate (Na2S2O3). The end
point of titration is indicated by the disappearance of blue color, produced by the reaction
between iodine and starch (which is added as indicator during the titration),
I2 + 2 Na2S2O3 = Na2S4O6 + 2 Nal
or, I2 + 2S2O32- = S4O62- + 2I-
I2 + starch = blue color
(Qualitative test for the presence of iodine/chlorine)
The titration is carried out at pH 3 to 4, because the reaction with thiosulfate is not
stoichiometric at neutral pH due to partial oxidation of the thiosulfate to sulphate.
73
Procedure for determination of residual chlorine concentration:
1. Place 200 mL of the sample in an Erlenmeyer flask.
2. Add 'about 1g of potassium iodide (estimated on a spatula) and 2 mL of concentrated
Acetic acid to the water.
3. Add 0.025 N sodium thiosulfate drop by drop from a burette until the yellow color almost
disappears.
4. Add 1 mL of starch solution to the water.
5. Continue addition of standard sodium thiosulfate (Na2S2O3) solution until the blue color
just disappears.
6. Record the quantity (in mL) of sodium thiosulfate (Na2S2O3) solution used.
Calculation:
M.F. =
Assignment:
1. What are the major disadvantages 'of chlorination? Name some of the alternate disinfectants.
2. You would like to perform chlorination to a water sample with pH 7.5. At this pH, what would be
the relative proportions of HOCl and OCI-? What kind of change in pH would you propose in
order to increase the relative proportion of HOCL, which is a better disinfectant?
3. Schematically draw “chlorine residual" versus "chlorine dose" curve for a water sample with no
ammonia or organic matter.
74
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
75
Experiment 15
Determination of Total and Fecal Coliform
in water
76
Introduction:
A variety of different microorganisms are found in untreated water. Most of these organisms
do not pose a health hazard to humans. Certain organisms, referred to as pathogens, cause
disease to humans which include species of bacteria, viruses and protozoa. These organisms
are not native to aquatic systems and usually require an animal host for growth and
reproduction. Pathogens are likely to gain entrance sporadically, and they do not survive for
very long period of time; consequently they could be missed in a sample submitted to the
laboratory. Although it is possible to detect the presence of various pathogens in water, the
isolation and identification of many of these is often extremely complicated, time-consuming
and expensive proposition. Hence in most cases (except when presence of any particular
microorganism is suspected) the microbiological quality of water is checked using some
indicator organisms.
An indicator organism is one whose presence presumes that contamination has occurred and
suggests the nature and extent of the contaminants. An indicator organism should be a
microorganism whose presence is evidence of fecal contamination of warm blooded animals.
Indicators may be accompanied by pathogens, but typically do not cause disease themselves.
The ideal indicator organism should have the following characteristics:
Total coliforms are defined as gram negative bacteria which ferment lactose at 35° or 37° C
with the production of acid, gas and aldehyde within 24 or 48 hours. Fecal coliform are a
subgroup of total coliforms, which live in the warm blooded animals and have the same
properties as thetotalcoliform but tolerate and grow at higher selective temperature range of
44° to 44.5°C. In addition, they form indole from tryptophan. And these combined properties,
when positive, are regarded as presumptive Escherichia coli (presumptive E. coli). Some
coliform species are frequently associated with plant debris or may be common inhabitants in
soil or surface waters which arc called non-fecal coliforms.
Apparatus:
1. Petri Dish
2. Incubator
3. Measuring Cylinder, beaker, dropper etc.
Reagents:
1. Appropriate culture medium (broth)
2. Distilled water
78
Advantages:
Results are obtained more quickly as the number of coliforms can be assessed in less
than 24 hours, whereas the multiple tube technique requires 48 hours both for a
negative or a presumptive positive test;
Saving in work, certain supplies and glassware;
Method gives direct results;
Easy to use in laboratories, or even in the field if portable equipment is used.
Disadvantages:
High turbidity caused by clay, algae, etc. prevents the filtration of a sufficient volume
of water for analysis and it may also produce a deposit on the membrane which could
interfere with bacterial growth;
Presence of a relatively high non-coliform count may interfere with the determination
of coliforms:
Waters containing particular toxic substances which may be absorbed by the
membranes, can affect the growth of the coliforms.
79
the colony. Colonies of other types should not be counted. The colonies can be counted with
the aid of a lens. The number of total coliforms per 100 mL is then given by:
Calculation:
Assignment:
1. What do you understand by "indicator organisms"? Why water samples are usually tested for
indicator organisms instead of specific pathogenic organisms?
2. Define and differentiate between total coliform (TC) and fecal coliform (FC)?
3. What are the major advantages of "membrane filtration method" over "multiple tube method"?
80
DATA SHEET
Experiment Name :
Experiment Date :
Student’s Name :
Student’s ID :
Year/ Semester :
Section :
Group :
Table
81
Sampling and Laboratory Analysis of Air
82
Ambient Air Sampling Guideline:
It includes-
- Survey for preliminary information
- Selection of sampling procedure
- Sampling locations
- Period of sampling, frequency and duration
Title:
Sampling of sulphur dioxide in ambient air and the determination of its concentration
Method of measurement:
Volumetric - sampling a volume of air through a collecting medium at a known flow rate for
a specified time.
Instrument:
Gas sampler of midget impingers or high volume sampler with a gas kit attachment for S02.
Auxiliaries:
Standard glass bubblers, airflow rotameter for measuring flow rate
Chemicals:
0.1 N Sodium tetra-chloromercurate, an absorbing reagent.
Sampling location guidelines:
Sampling station should be located depending upon the objective of measurement campaign
and be kept at an altitude depending upon the type of study region (roadways, industrial area,
disposal sites, residential tract, etc). Generally it is kept at a height of about 3 to 10 m from
the ground level and sufficiently away from the disturbance or direct obstacle from the source
under consideration.
84
Chemicals:
Pararosaniline hydrochloride
Acid bleached
Formaldehyde (0.2%)
Sulphamic acid by dissolving 0.8 g in 100 ml distilled water
Standard sulphur dioxide solution by dissolving 004g sodium
metabisulphite in 250 ml distilled water
Steps of analysis:
Calibration curve:
Prepare a standard solution of S02 concentrations ranging from 0 to 25 micro gram
S02 by taking definite amounts of std. sulphur dioxide solution in a 25 ml volumetric
flasks
Add 14 ml of absorbing reagent and 1 ml of pararosaniline hydrochloride to each of
the flasks making a total volume of 20 ml.
Measure absorbance for each flasks by spectrophotometer at 540 nm wavelength
Plot graph of absorbance vi concentration
Absorbance in samples:
Transfer samples to a 25 ml flask and develop colour as done in calibration curve
Measure absorbance at 540 nm
Find out the concentration (micro gram S02) corresponding to the measured
absorbance from the calibration curve
Calculations:
1. Average flow rate (if there is a significant difference in initial and final flow rates)
2. Total volume of air sampled (TVA) in m3 = Avg. flow rate (lit)" 10-3 (me/lit) * time
(hr) * 60 (rnin/hr)
3. Micro gram S02 /TVA
Oxide of Nitrogen:
Title:
Sampling of oxides of nitrogen In ambient air and the determination of its concentration
Method of measurement:
Volumetric - sampling a volume of air through a collecting medium at a known flow rate for
a specified time.
Instrument:
Gas sampler of midget impingers or high volume sampler with a gas kit attachment for NOx
Auxiliaries:
Standard glass bubblers, airflow rotameter for measuring flow rate
Chemicals:
Solution of sodium hydroxide and sodium arsenite, an absorbing reagent
Sampling location guidelines:
Sampling station should be located depending upon the objective of measurement campaign
and be kept at an altitude depending upon the type of study region (roadways, industrial area,
disposal sites, residential tract, etc). Generally it is kept at a height of about 3 to 10 m from
the ground level and sufficiently away from the disturbance or direct obstacle from the source
under consideration.
Sampling frequency guidelines:
Sampling is carried out for various purposes. The regular monitoring campaign of national
ambient air quality includes measurement of NOx typically for 24 hours at least twice a week
making about 104 samples a year.
85
Steps for sampling:
Prepare absorbing reagent (a solution of sodium hydroxide and arsenite) by dissolving
4 g sodium hydroxide and 1 g of sodium arsenite in 1 lit of distilled water
Prepare a sampling train of at least 2 gas bubblers (for average reading) properly
washed with distilled water and air dried.
Place bubblers in the sampling system securely connecting to the manifold. Check the
connections of bubblers with the manifold and the inlet and outlet
Fill the bubblers with an absorbing reagent with an amount sufficient to last for 24
hours (approximately 15 ml for 8 hours sampling to 50 ml for 24 hours sampling)
To eliminate interferences of sulphur dioxide, drop of hydrogen peroxide may be
added to the reagent to convert sulphur dioxide into sulphate during analysis
Start the sampler and adjust flow rate to about 0.2 lit/rnin for 24 hours sampling
Note the flow rate at the end of the desired sampling period and stop the sampler
Transit the sampling train to environmental laboratory carefully with scientific
precautions and preserve the sample tubes in a controlled environmental conditions
Laboratory analysis:
Method:
Colorimetric - by reacting the nitrite ions with phosphorus acid, sulphanilamide, and NEDA
solution by measuring absorbance of NOx from the exposed absorbing reagent at 540 nm
using spectrophotometer.
Chemicals:
Hydrogen peroxide solution
N-(I-Napthyl)-ethylenediamine Di-hydrochloride (NEDA)
Sodium nitrite - assay of NaN02 (=> 97 %)
Sodium nitrite stock solution (1000 μg N02/ml)
Sodium nitrite solution (10 μg N02/ml)
Sodium nitrite solution (1 μg N02/ml)
Sulphanilamide solution
Phosphoric acid
Steps of analysis:
Calibration curve:
Prepare a standard solution of NOx concentrations ranging from 0 to 25 μg S02 by
taking definite amounts of std. sulphur dioxide solution in a 25 ml volumetric flasks
Add 14 ml of absorbing reagent and 1 ml of pararosaniline hydrochloride to each of
the flasks making a total volume of 20 ml.
Measure absorbance for each flasks by spectrophotometer at 540 nm wavelength
Plot graph of absorbance via concentration
Absorbance in exposed samples:
Transfer samples to a 25 ml flask and develop colour as done in calibration curve
Measure absorbance at 540 nm
Calculations:
1. Average flow rate (if there is a significant difference in initial and final flow rates)
Average flow rate (initial and final flow rates) in lit/min. = (Initial flow rate + final
flow rate/2
2. Total volume of air sampled (TVA) in m3 = = Avg. flow rate (lit/min)* 10-3(m3/lit) *
sampling time (hr) * 60 (min/hr)
86
Particulate matter:
Title:
Sampling of suspended particulate matter in ambient air and the determination of its
concentration
Method of measurement:
Volumetric-filtration - sampling a volume of air through a filter medium at a known flow rate
for a specified time.
Instrument:
High volume sampler with SPM filter manifold
Auxiliaries:
High volume sampler with airflow manometer for measuring flow rate, microfiber filter (8" x
10" size)
Sampling location guidelines:
Sampling station should be located depending upon the objective of measurement campaign
and be kept at an altitude depending upon the type of study region (roadways, industrial area,
disposal sites, residential tract, etc). Generally it is kept at a height of about 3 to 10 m from
the ground level and sufficiently away from the disturbance
Sampling frequency guidelines:
Sampling is carried out for various purposes. The regular monitoring campaign of national
ambient air quality includes measurement of SPM typically for 24 hours at least twice a week
making about 104 samples a year.
Steps for sampling:
Condition a filter paper in oven
Prepare a sampling assembly by uncorking screws of the bracket.
Take the tare (initial) weight of filter paper (Wi, mg)
Place the filter in the sampling system securely and tighten the screws of the bracket.
Set the timer for the period of sampling
Start the sampler and adjust flow rate to about 2 lit/rnin for 24 hours sampling.
Note the flow rate at the end of the desired sampling period and stop the sampler
Transit the sampling train to environmental laboratory carefully with scientific
precautions
Condition the filter paper again for the same period as was done prior to sampling
Laboratory analysis:
Method:
Gravimetric - by weighing the mass of particles
Steps of analysis:
Weighing of exposed samples:
Take final weight of the exposed filter with a standard balance (WI, mg)
Calculations:
1. Average flow rate (initial and final flow rates) in lit/min. = (Initial flow rate + final
flow rate/2
2. Total volume of air sampled (TVA) in m3 = Avg. flow rate (lit/min)* 10-3(m3/lit) *
sampling time (hr) * 60 (min/hr)
3. Concentration of SPM in μg/m3 = ( wf- wi) ( mg)/ TVA (m3)*106 g/m3
87
Sampling and Laboratory Analysis of Solid Waste
88
Guidance for carrying out waste sampling and analysis
Depending on the needs of the client analysis of waste may have different objectives. For
instance, waste producers want to know what kind of recovery/disposal is possible, managers
of waste treatment plants need to know if they can accept and will be able to treat the waste
and authorities are interested in the environmental effects related to a particular waste. The
different needs of the concerned actors lead to different testing programmes in which sample
taking is required. The strategy of sampling and analysis has to be planned in advance very
carefully in order to avoid useless efforts and unnecessary costs. The correct procedure of
sampling is very important to get a representative sample of the specific waste subject to
testing. A representative sample of a specific waste is important to ensure the reliability of
analysis results obtained, which is the decision basis for the subsequent choice of waste
management operations and handling.
90
Appendix 1
The Environment Conservation Rules, 1997
Notes:
1. In water used for pisiculture, maximum limit of presence of ammonia as Nitrogen is
1.2 mg/l.
2. Electrical conductivity for irrigation water – 2250 µmhoms/cm (at a temperature of
25°C); Sodium less than 26%; boron less than 0.2%.
91
92
93
Notes:
1. At national level, sensitive area includes monuments, health center, hospital, archeological
site, educational institution, and government designated areas (if any).
2. Industrial units located in areas not designated as industrial areas shall not discharge
pollutants which may contribute to exceeding the standard for air surrounding the areas
specified at Sl. nos. c and d above.
3. Suspended Particulate Matter means airborne particles of adiameter of 10 micron or less.
94
Notes:
1. This limit shall be applicable to discharges into surface and inland waters bodies.
2. Sewage shall be chlorinated before final discharge.
95
96
97
Notes:
1. These standards shall be applicable to all industries or projects other than those
specified under the heading “Standards for sector wise industrial effluent or
emission.”
2. Compliance with these standards shall be ensured from the moment an industrial unit
starts trial production, and in other cases, from the project starts operation.
3. These standards shall be inviolable even in case of any sample collected instantly at
any point of time. These standards may be enforced in a more stringent manner if
considered necessary in view of the environmental conditions of a particular situation.
4. Inland Surface Water means drains/ponds/tanks/water bodies/ditches, canals, rivers,
springs and estuaries.
5. Public sewerage system means treatment facilities of the first and second stage and
also the combined and complete treatment facilities.
6. Irrigable land means such land area which is sufficiently irrigated by waste water
taking into consideration the quantity and quality of such water for cultivation of
selected crops on that land.
7. Inland Surface Water Standards shall apply to any discharge to a public sewerage
system or to land if the discharge does not meet the requirements of the definitions in
notes 5 and 6 above.
98
Appendix 2
Lab Report Format
1. All students must have a same colored printed cover page. The design of cover page
is provided with the lab manual. Students have to compose only the course teacher’s
name and designation ant their information.
2. An index is provided. It should be printed and set after the cover page. Table may be
fill up by pen during each submission after test.
3. Each report must have a common printed top page. Only the experiment name and
no. and the date may be filled up by pen. A top page design is provided.
4. A4 papers have to be used for preparing the lab report. Writing should be done with
pen. Pencil may be used for any kind of sketch.
5. In each experiment of the lab report the following points must have to be present:
Objective, Equipment, Procedure, Data Table (signed), Sample Calculation,
Result and Discussion.
99
INDEX
Sl. Name of The Date of Date of Signature Comments Page
No. Experiment/ Performance Submission no.
Assignment
100
References
1. “Standard Methods for the Examination of Water and Waste Water”, American Public Health
Association, APHA, 20th Edition, 1995.
2. “The Environment Conservation Rules", 1997.
3. “The Environmental Conservation Act”, 1995.