Environmental Engg. 3160611 - Lab Manual
Environmental Engg. 3160611 - Lab Manual
Environmental Engg. 3160611 - Lab Manual
Subject Coordinators:
Dr. Manjurali I. Balya
Assistant Professor
Civil Engineering Department
CIVIL ENGINEERING DEPARTMENT
GOVERNMENT ENGINEERING COLLEGE, PATAN
CERTIFICATE
This is to certify that the bonafide record of work done by
Mr./Miss……..……………………………………………………………………
Bearing Enrollment No. ……….……….. is a student 6th semester in Civil
Engineering branch has completed Laboratory of course Environmental
Engineering (3160611) during the Academic year……………………
……………………………….
Signature of Faculty-In-charge
………………..
Signature of HOD
INDEX
Sr. Hrs (CO
Title of Experiment Date Grade Sign.
No. addressed)
Introduction to Equipment in
1 Environmental Engineering
Laboratory
Introduction to Standards,
2 Sampling, Collection &
Preservation of Samples
Determination of pH &
3 Conductivity for water &
wastewater
Determination of Solids
4 (suspended, dissolved and
settleable)
Determination Acidity,
5
Alkalinity and Hardness
Determination Chloride and
6
Residual Chlorine
Exhaust gas analysis for air
7
pollutants
Measurement of noise at
8 different sources using Sound
meter
Introduction to Equipment in Environmental
Practical No. 1
Engineering Laboratory
❖ Introduction
A well equipped laboratory is a prerequisites for efficient analytical control .The size and
equipment of the laboratory depend s more upon the nature of the processes to be controlled and
to a lesser extent on the size of the plant .the laboratory could be divide in to several units; viz; a
physical and chemicals laboratory, a bacteriological laboratory biological laboratory, a biological
laboratory, a preparation room and a store.
The equipment in the laboratory must be adequate to permit the proper analytical laboratory control
of Purification processes. Careful planning is necessary while equipping the laboratory to effect
proper utilization Of the equipments. The proper maintenance of equipments and storage of
chemicals must be in the hand of Responsible analyst .A need-based planning to acquire
consumable materials like glassware, chemicals And reagents is generally more important than the
procurement of various special equipments. Calibrated Instruments should frequently be checked
using standards.
❖ Different laboratory equipments and instruments are used for analysis and
performances of practical works are:
7. Dissolved Oxygen Meter 17. PM2.5 & PM10 Combo Air Sampler
1. Standards
There are certain primary standards which are related to human health and certain
secondary standards which are related to protect human welfare. For water quality
monitoring study, three standards are of interest:
Ask yourself the purpose of study (?), what data are needed (?) and then select
most suitable location that can provide the required information.
Site location for river
• Upstream of the industrial and domestic discharge points
• Immediately downstream of industrial and domestic discharge points.
• At a place of abstraction for industrial use and public water supply.
• Base line stations where water is available in natural state.
Grab Samples
A sample collected at a particular time and place can represent only the
composition of the source at that time and place. It shows only the prevailing
conditions at the time of sampling and does not represent the average conditions.
Sampling of water from sources such as wells, rivers, streams, lakes, oceans and
reservoir for chemical, physical and bacteriological analysis.
• When a source is known to be constant over a considerable time period, in that
case a single grab sample should be considered as representative.
• If the sources are known to vary with time, grab sample should be collected at
suitable intervals of time and analyzed separately.
• The results can be documented in terms of mean, standard deviation, frequency,
and duration of variations. When the source composition varies in space (in
different locations), collect samples from appropriate locations.
Composite Samples
The term composite refers to a mixture of grab samples collected at the same
sampling point at different times. A composite sample of 24 h period is considered
standard for most of the determination. It provides more meaningful data than the
grab samples.
Integrated Samples
They represent the mixture of grab samples collected from different points
simultaneously and mixed in equal volumes.
• Such samples are useful for rivers or streams that vary in composition across the width
and depth. For collection of integrated samples, special sampling device is needed.
• Sample is collected at a known depth without disturbing the surface water.
The sampling bottle may be made of either glass or plastic, usually polyethylene.
It must be capable of being tightly sealed either by stopper or cap.
• The bottles should be soaked with 10% HCI for 24 h and then thoroughly cleaned and
rinsed with distilled water.
• Cleaning solution; acid dichromate: Prepare a saturated water solution of potassium
dichromate (K 2Cr 2O 7). Add 32 mL of this K 2Cr 2O 7 solution in 1L of concentrated
H 2SO 4 (sp. gr. 1.84).
Each sampling bottle must be provided with an identification label on which the
following information is legibly and indelibly written (Given below Table).
1. Name of Study :
5. Volume of sample :
Recommended
Parameter Recommended Preservation Maximum
Sample
Container Method Storage Time
Volume (ml)
Acidity 100 P or G 40C 24 hours
Alkalinity 200 P or G 40C 24 hours
BOD 1000 P or G 40C 6 hours
P or G Analyses as soon as
COD 100 possible or add 7 days
conc. H2SO 4 to
pH<2
Conductivity 500 P or G 40C 28 days
Sulphate 100 P or G 40C 28 days
Solids 100 P or G 40C 7 days
Chlorine P or G Analyze Immediately
500 0.5 hours
Residual
Flouride 500 P Not required 28 days
P or G Add HNO 3 to
Hardness 100 6 months
pH<2
Nitrate 100 P or G 40C 48 hours
P or G Analyze
Nitrite 200 -
Immediately
-
pH 100 P or G --do-- 2 hours
Temperature 100 P or G --do-- -
-
DO 300 G --do-- 6 hours
Phosphate 100 G 100 C 48 hours
Analyze same
Turbidity 100 P or G day, store in 24 hours
dark up to 24
hours
P-Plastic or G- Glass
PH
Aim: To determine the pH of the given sample.
Theory: pH of aqueous solutions can be defined as negative logarithm of hydrogen ion
concentration. pH values ranging from 0 to 7 are acidic, and from 7 to 14 are alkaline.
The effect of pH on the chemical and biological properties of liquids makes its
determination very important. It is used in several calculations in analytical work.
The pH determination is usually done by electrometric method which is the most accurate
method and free of interference.
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.
Dewatering of sludge, oxidation of cyanides and reduction of Haxavalent chromium
into trivalent chromium also need a favorable pH range. It is used in the calculation
of carbonate, bicarbonate, CO 2 corrosion, stability index and acid base equilibrium.
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
trihaloethanes, which are causing cancer in human beings.
Electrometric Method:
The pH is determined by measurement of the electromotive force of a cell comprising
an indicator electrode (an electrode responsive to hydrogen ions such as glass
electrode) immersed in the test solution and a reference electrode or a combined
electrode. The contact between the test solution and the reference electrode is usually
achieved by means of a liquid junction. The emf of this cell is measured with pH
meter. This is a high impedance electrometer calibrated in terms of pH.
Reagents: Calibrates the electrode system against standard buffer solution of known pH.
Buffer tablets having pH 4.0, 7.0 and 9.2 are available.
Reagents:
Procedure:
1. Prepare buffers of pH 4, 7 and 9.2.
2. Rinse the electrode thoroughly with distilled water.
3. Standardize pH meter electrode with any two of these buffers.
4. Dip the electrode in the sample for test.
5. Let the reading on screen stabilize; note it as pH & temperature of your sample.
Results:
Theory: Conductivity is the capacity of water to carry an electrical current and varies
both with number and types of ions the solution contains, which in turn is related to
the concentration of ionized substances in the water. Most dissolved inorganic
substances in water are in the ionized form and hence contribute to conductance.
Conductivity measurement gives rapid and practical estimate of the variations in the
dissolved contents of water.
Environmental Significance:
Electrical conductivity measurements are often employed to monitor desalination
plants. It is useful for detection of impurities in water. Used for quantitative
measurement of ionic constituents dissolved in water, which are important for boiler
feed water and cooling water etc.; Used for checking correctness of water analysis as
there is a distinct relationship between conductivity and total dissolved solids (TDS).
Conductivity data is useful in determining the suitability of water and wastewater for
disposal on land. Irrigation waters up to 2 millisiemens/cm conductance have been
found to be suitable for irrigation depending on soils and climatic characteristics.
Reagents:
0.01 N, KCL solution: Dissolve 0.746 grams of potassium chloride in 1 liter of
distilled water.
Procedure:
1. Rinse the electrode thoroughly blots and dry.
2. Immerse the electrode in 0.01 N KCL solutions and the conductivity should be
1413 micro mhos at 25°C Temperature.
3. Now the instrument is calibrated.
4. Remove the cell from KCL solution and wash it thoroughly with distilled
water.
5. Immerse the electrode/cell in the unknown sample whose conductivity is to be
determined.
6. Note down the instrument reading. If the cell constant is given on the cell itself,
then the measured value of conductivity = Cell Constant C X Screen reading
Results:
Environmental Significance:
• They cut down light transmission through the water and so lower the rate of
photosynthesis in aquatic flora.
• In less turbulent parts of river, some of the solids may sediment out, smothering life of
the riverbed.
• The TSS determination is extremely valuable in the analysis of polluted water.
• It is a major parameter used to evaluate the strength of domestic wastewater and to
determine the efficiency of treatment unit.
Procedure:
1. Measure the empty weight of filter paper and note down reading. (Wi)
2. Mix Sample well and pour into a graduated cylinder to the selected volume. (V )
3. Apply suction to filter flask and seat filter with a small amount of distilled water.
4. Pour selected volume into filtration apparatus.
5. Wash with 3-successive 10-mL volume of distilled water, allowing complete
drainage between washing, and continue suction for about 3 minutes after filtration
is completed.
6. Carefully remove the filter paper from filtration apparatus and transfer it to an
weighing dish as a support.
7. Dry for at least 1 hour at 103-105°C in a hot air oven.
8. Cool in desiccator and weigh filter paper and record the reading (Wf)
9. Repeat cycle of drying, cooling, desiccating and weighing until a constant weight
is obtained, or weight change is less than 4% of previous weight or 0.5 mg,
whichever is less. Duplicate determination should be within 5% of their average.
Observation:
Sr. Water Waste water
Particular
No. Sample Sample
1. Initial Wight of Filter Paper in gm, (Wi)
2. Final Wight of Filter Paper in gm, (Wf)
3. Total Wight of Filter Paper in gm, (W)
4. Volume of Sample in ml, (V)
Calculation:
Aim: To determine the Dissolved solids present in water sample & waste water.
Environmental Significance:
• They A high content of dissolved solids elevates the density of water, influences
osmoregulation of freshwater organisms, reduces solubility of gases (like oxygen) and
reduces utility of water for drinking, irrigation and industrial purposes.
• TDS concentration beyond 500 mg/L, decreases palatability and may cause
gastrointestinal irritation.
Procedure:
1. Take a clean porcelain dish/beaker which has been washed and dried in a hot air
oven at 103-105 °C for one hour.
2. Now weigh the empty porcelain dish/beaker in analytical balance. (Wi)
3. Mix sample well and pour into a funnel with filter paper. Filter a known volume
of a well-mixed sample in the above beaker. (i.e. 100 mL, 200 mL or 500 mL) (V)
4. Note: Choose the sample volume to yield 10 to 200 mg of dried residue. If more
than 10 minutes are required for complete filtration, decrease the sample volume.
5. Evaporate the sample in a hot air over at180 ± 2 °C after the whole water is
evaporated, cool the evaporating dish/beaker in a desiccator and take the final
weight (Wf).
6. Total solids = (Suspended solids) + (Dissolved solids).
Observation:
Sr. Waste water
No. Particular Water Sample
Sample
1. Initial Wight of Beaker in gm, (Wi)
Theory: The term settleable solids are applied to the solids in suspension that will settle,
under quiescent conditions, because of the influence of gravity. Only the coarser
suspended solids with a specific gravity sufficiently greater tha n that of water settle.
Sludge is accumulation of settleable solids. Settleable solids may be determined and
reported on either a volume (mL/L) or a weight (mg/L) basis.
Environmental Significance:
• To determine the need for and design of primary settling tank.
• To determine the efficiency of sedimentation units.
• To study the physical behavior of waste streams entering natural water bodies.
Volumetric Method:
Procedure:
1. Fill an Imhoff cone to the l-L mark with a well-mixed sample).
2. Settle for 4S-min, gently agitate sample near the sides of the cone with a rod or by
spinning, settle 15 min longer, and record volume of settleable solids in the cone as
mL/L.
3. If the settled matter contains pockets of liquid between large settled particles,
estimate volume of these and subtract from volume of settled solids.
4. The practical lower limit of measurement depends on sample composition and
generally is in the range of 0.1 to 1.0 mL/L. where a separation of settleable and
floating materials occurs, do not estimate the floating material as settleable matter.
5. Replicates usually are not required.
Results:
Report the results as mL of settleable solids/L (volumetric method).
Gravimetric Method:
Procedure:
1. Determine the total suspended solids (TSS) as given above (page 20).
2. Determination of non-settleable solids is as follows.
3. Take 1 L measuring cylinder and pour about 1 L of sample (Note: the
minimum depth of sample should be 20 cm).
4. Let stand quiescent for 1h and, without disturbing the settled or floating material,
siphon 2S0mL from center of measuring cylinder at a halfway between the surface
of the settled material and the liquid surface.
5. Determine total suspended solids (mg/L) of this supernatant liquor. These are
the non-settleable solids.
Calculation
ACIDITY
Aim: To determine the acidity present in water & Wastewater sample
Environmental Significance:
• Acidity is interferes in the treatment of water. Carbon dioxide is of important
considerations in determining whether removal by aeration or simple neutralization
with lime / lime soda ash or NaOH will be chosen as the water treatment method.
• The size of the equipment, chemical requirements, storage spaces and cost of the
treatment all depends on the carbon dioxide present.
• Aquatic life is affected by high water acidity. The organisms present are prone to
death with low pH of water.
• High acidity water is not used for construction purposes. Especially in reinforced
concrete construction due to the corrosive nature of high acidity water.
• Water containing mineral acidity is not fit for drinking purposes.
• Industrial wastewaters containing high mineral acidity is must be neutralized
before they are subjected to biological treatment or direct discharge to water sources.
Apparatus: Titration Stand with Burette, Conical Flask, Beaker, Measuring Cylinder,
Pipette, Funnel, Wash Bottle etc.
Reagents:
o N NaOH Solution: Dissolve 0.8 grams of NaOH in 1 liter of distilled water.
• Phenolphthalein Indicator: Dissolve 0.5 gm of Phenolphthalein Indicator in 500
ml95% of ethyl alcohol. Add 500 mL distilled water.
• Methyl orange Indicator: Dissolve 0.5 g of Methyl orange Indicator & dilute to
1000 ml with distilled water.
Procedure:
A. Methyl Orange Acidity
B. Phenolphthalein Acidity
Observation:
1. Titrant :
2. Indicators : Phenolphthalein and Methyl Orange Indicator
3. End Point: a) Yellow to Faint Orange
b) Colorless to Faint Pink Color
Table: 1 Mineral Acidity: (Methyl Orange Indicator)
Calculations:
Volume of NaOH (A) x N x 50 x 1000
Mineral Acidity as CaCO 3 in = V
mg/L
Results:
Mineral Acidity Phenolphthalein Total
Sample Used Acidity
(mg/L) Acidity (mg/L)
(mg/L)
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 in waters. The resultant precipitate can corrode pi pes 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.
• The alkalinity acts as a pH buffer in coagulation and lime-soda softening of water.
• In wastewater treatment, alkalinity is an important parameter in determining the
amenability of wastes to the treatment process and control of processes such as
anaerobic digestion, where bicarbonate alkalinity, and any fraction contributed by
volatile acid salts become considerations.
Apparatus: Titration Stand with Burette, Conical Flask, Beaker, Measuring Cylinder,
Pipette, Funnel, Wash Bottle etc.
Reagents:
• 0.02N H2SO4: 3 mL. Conc. H2SO4 in 1 L distilled water to get 0.01 N H2SO4. Take
100 mL 0.01 N H2SO4 + 500 mL distilled water
• Phenolphthalein Indicator: Dissolve 0.5 gm of Phenolphthalein Indicator in 500 ml
95% of ethyl alcohol. Add 500 mL distilled water.
• Methyl orange Indicator: Dissolve 0.5 g of Methyl orange Indicator & dilute to
1000 ml with distilled water.
Procedure:
A. Phenolphthalein Alkalinity:
1. Take suitable volume of sample (25, 50 or 100 mL) in a conical flask.
2. Add 2-3 drops of phenolphthalein indicator.
3. If the sample turns pink in color, then titrate with 0.02 NH2SO4, till the pink color
disappears. Note the volume of acid required as (A).
4. If the pink color does not exist it indicates that, phenolphthalein Alkalinity is
absent. Then continue the titration with Methyl Orange indicator.
1. Titrant :
2. Indicators : Phenolphthalein and Methyl Orange Indicator
3. End Point: a) Pink to Colorless
b) Yellow to Faint Orange Color
Calculations:
Results:
Sample Used
Phenolphthalein
Alkalinity (mg/L)
Methyl Orange
Alkalinity (mg/L)
Total Alkalinity (mg/L)
Hydroxide
Alkalinity
Carbonate
Alkalinity
Bicarbonate
Alkalinity
A small amount of dye Erichrome Black –T is added to hard water containing Calcium
and Magnesium ion, the solution will become wine red. EDTA is then added as a titrant.
Complexes of Calcium and Magnesium are formed after sufficient EDTA has been added.
The solution turns from Wine Red to Blue. This is the end point of titration, a pH value
of 10.2 is usually maintained.
The degree of hardness of drinking water has been classified in terms of the
equivalent CaCO 3 concentration as follows:
Soft: 0 - 60 mg/L.
Medium: 60 - 120 mg/L.
Hard: 120 -180 mg/L
Very hard: > 180 mg/L.
Environmental Significance:
• Scales are formed as inner coating of the pipelines prevents corrosion.
• Absolutely soft waters are corrosive and dissolve the metals.
• More cases of cardio vascular diseases are reported in soft water areas.
• Hard water is useful to growth of children due to the presence of calcium.
• Hard waters cause excessive consumption of soap used for cleaning purpose. Sodium
soaps react with multivalent metallic cations to form a precipitate, thereby lose their
surfactant properties. Lathering doesn’t take place until all hardness ions precipitate
out.
• This precipitate adheres to surfaces of tubes, sinks, dish washer and may stain
clothing.
• Scales formed mainly due to carbonate hardness act as insulations and cause
enormous loss of fuel in boiler.
• Scales deposited mainly due to increase in pH to 9 at which bicarbonates are
converted as carbonates are formed in distribution mains reducing their carrying
capacity.
Procedure:
• Take well mixed suitable volume of sample (25, 50 or 100 mL) in a conical flask (V).
Select a sample volume that requires less than 15 mL EDTA titrant and complete
titration within 5 minutes, measured from time of buffer addition.
• Add 1-2 ml of Ammonia buffer solution. Usually 1-2 mL buffer solution is sufficient
to give a pH of 10.0 to 10.1 and mix well.
• Add a pinch of Erichrome black T and titrate with standard EDTA (0.01 M) till wine
red color changes to blue color. Note down the Volume of EDTA required. (A).
• Run a reagent blank with distilled water. Note the volume of EDTA consumed (B).
• Calculate the volume of EDTA required by sample; C = (A-B)
Observation:
1. Titrant :
2. Indicators : Eriochrome Black T Indicator
3. End Point : Wine Red to Blue
Burette Reading Burette Reading
Volume Volume of
Sr. of Sample; A of Blank; B
of Sample; (ml) (ml) EDTA
No.
V (ml) (ml) (C=A-
Initial Final Total Initial Final Total B)
Calculations:
Results:
CHLORIDE
Aim: To determine the chloride content of the given water sample by Mohr's method
Theory: Chloride in the form of Chlorine ion is one of the major inorganic anions. The
salty taste produced by Chloride concentration is variable and dependent on the chemical
composition of water. The Chloride is higher in wastewater than in raw water. Along t he
sea costal, Chloride may be present in high concentrations because of intrusion of salt
water into the water and sewage system. In this method, slightly alkaline solution is used.
Potassium chromate can indicate the end point of Silver nitrate titration of Chloride as
quantitatively precipitated before red Silver chromate is formed.
Environmental Significance:
• Chlorides associated with sodium (Sodium Chloride) exert salty taste when its
concentration is more than 250 mg/L. These impact a salty taste to water. Chlorides
are generally limited to 250 mg/L in water supplies intended for public water supply.
• In many arrears of the world where water supplies are scarce, sources containing as
much as 2000 mg/L are used for domestic purposes without the developm ent of
adverse effect, once the human system becomes adapted to the water.
• It can also corrode concrete. Magnesium chloride in water generates hydrochloric
acid after heating which is also highly corrosive and creates problem in boilers.
• Chloride determinations in natural waters are useful in the selection of water supplies
for human use.
• Chloride determination is used to determine the type of desalting apparatus to be
used.
• Chloride determination is used to control pumping of ground water from locations
where intrusion of seawater is a problem.
Apparatus: Titration Stand with Burette, Conical Flask, Beaker, Measuring Cylinder,
Pipette, Funnel, Wash Bottle etc.
Reagents:
• Standard Silver nitrate titrant (0.0141 N): Dissolve 2.395 gm of silver
nitrate in distilled water and dilute to 1000 ml. Standardize against 0.0141
N sodium chloride solution.
• Standard sodium chloride solution (0.0141 N): Dissolve 824 mg of sodium chloride
(Dried) in distilled water and dilute to 1 litre. 1 ml = 500 µg of chloride.
• Potassium chromate indicator solution: Dissolve 50 gm of potassium chromate in
a little distilled water. Add few drops of silver nitrate solution until a definite red
precipitate is formed. Let it stand for 12 hour, filter and dilute to 1 litre with distilled
water.
Procedure:
1. Take well mixed suitable volume of sample (25, 50 or 100 mL) in a conical flask
(V).
2. Add 1ml of potassium Chromate indicator. The color of the solution turns to yellow
color.
3. Titrate against Standard silver Nitrate solution till color change from yellow to
brick red.
4. Note the Burette volume of silver Nitrate added (A)
5. For better accuracy, titrate distilled water (blank) in the same m anner. Note the
burette volume of silver Nitrate added for distilled water (B).
6. Calculate the volume of EDTA required by sample; C = (A -B)
Observation:
1. Titrant :
2. Indicators : Potassium Chromate Solution
3. End Point : Yellow to Brick Red
Calculations:
Results:
Sampl Chloride in
e mg/L
Theory: Chlorine will liberate free iodine from potassium iodine (Kl) solutions at pH 8
or less. The liberated iodine is titrated with a standard solution of sodium thiosulphate
(Na2S2O3) with starch as the indicator. The liberated iodine is directly proportional to
the concentration of chlorine present in sample. Titrate at pH 3 to 4 because the reaction
is not stoichiometric at neutral pH due to partial oxidation of thiosulphate to sulphate.
Select a sample volume that will require not more than 20mL 0.01N sodium thiosulphate.
For residual chlorine concentration of 1 mg/L or less, 100mL sample for chlorine range
1-10 mg/L, 500ml for chlorine above 10mg/L and proportionally less as per chlorine
concentration.
Apparatus: Titration Stand with Burette, Conical Flask, Beaker, Measuring Cylinder,
Pipette, Funnel, Wash Bottle etc.
Reagents
Procedure:
1. Volume of sample: Select volume that will require not more than 20 ml. 0.01N
Na2 S2 O 3 and not less than 0.2 ml for the starch-iodide end point. For a
chlorine range of 1 to 10 mg/L, take 200 ml of chlorinated water sample in a
conical flask (V).
2. Add 5 ml Acetic Acid and mix well. To acidify the sample. It is used to reduce
the pH between 2 and 4 in the conical flask.
3. Add about 1 gm potassium Iodide (KI) measured using the spatula and dissolved
it by thoroughly mixing it with stirring rod. Perform the titration quickly, since
Iodine liberate faster.
4. Titrate the solution with standard Na 2 S2O 3 solution until the yellow colour of
librated iodine is almost faded out. (Pale yellow colour appears)
5. Add 1 ml of starch solution, the yellow colour changes to dark blue colour,
continue the titration until the blue colour disappears. Note Down the volume
of titrant used (A).
6. In many cases residual chlorine is very low and starch needed to be added
before starting up the titration.
Observation:
1. Titrant :
2. Indicators : Starch Solution
3. End Point: : Blue to Colorless
Sr. Volume of Sample (ml) (V) Burette Reading (ml) Volume of Na2S 2O3 (ml) (A)
No. Initial Final
Calculation:
Results:
• ABSTRACT:
Air pollution exists where there are quantitative variations in the air composition or by the
introducing of new pollutants. Air pollution is a major concern worldwide. It causes degradation
of ecosystems, giving rise to the greenhouse effect, to climate change, the decrease in air quality
and health problems in living beings. In extreme case, the gases constituents of the atmosphere, in
certain concentrations can cause death of persons, either by poisoning or by violence, they can
cause accidents. With the automobiles and industrialization increase there has been a need to
control gas emissions before loading them into the environment. To this end, environmental and
pollutants gas analyzers are used and it is necessary their calibration by competent entities. The
main proposal of this communication is to demonstrate the importance of the calibration operation
of these instruments as well as the calculation of associated uncertainties.
• INTRODUCTION :
Reference Gas Laboratory of IPQ is responsible for environmental and pollutants gas analyzers
calibration and for exhaust gas analyzers metrological control.The gas analyzers are measurement
instruments that detect the variation of gas concentration in the air omposition in places where they
are installed. This measurement instrument leads to a significant control of gaseous emissions to
protect people and surveilling toxic gases properties and/or fuels. The professional limits of
exposure (ELV) to chemical agents, pollutants and environmental gases are set, in Portugal, by the
Portuguese standard NP 1796/2004 [1]. Like other European Union countries, they are based on
the limits proposed by the American Conference of Governmental Industrial Hygienists (ACGIH),
2006. The Portuguese law is the transposition into of the Directive nº 96/62/CE, that establishes
measurements and procedures adequate to the pollution prevention and control from installations
responsible for the pollutants discharge into the air. It establishes also a monitoring system. Finally,
the Portuguese law sets the maximum and minimum mass thresholds applied to all emissions
sources [2, 3].
• ANALYZERS CALIBRATION
The standards used in analyzers calibration are certified reference mixtures traceable to IPQ and
VSL (Netherlands) standards. The preparation of primary gas mixtures and certification of
reference materials is performed at the highest metrological level, using methods based on ISO
international standards [4, 5].
Approval instrument:
When the errors observed for each reading are within the maximum permissible errors (EMA)
set in OIML R99 [8].
• CALCULATION OF UNCERTAINTY:
The uncertainties have been calculated in accordance with the "Guide to the expression of
uncertainty of measurement in calibration laboratories" [10].
The uncertainty component related to the dispersion of results is calculated using the of the
standard deviation of the mean of the measurements:
U disp =s (q ) /√u
Where s(q) is the standard deviation and n is the number of readings. The uncertainty
component related to the resolution of the analyzer is given by:
U div =resolution/√12
The uncertainty component of the used reference material is related to the uncertainty of
certified gas mixture and is given by the half of the expanded uncertainty of the standard:
𝑢
U padr = 2
• CONCLUSIONS :
The analysis of Fig. 3 and 4, for results of carbon monoxide analyzer and pollutants gas
analyzers respectively, evidence that the analyzer after the adjustment meets the metrological
criterion, for which was issued a calibration certificate.
The results of the exhaust gas analyzers show that the analyzer was approved because the
averages of the measured values were within the maximum permissible errors.
Practical No. 8 Measurement of noise at different sources using Sound meter
Theory: Noise level measurement procedure are processes which are followed while monitoring
sound level or acoustic energy level in specified area. These days annoying noise levels have
started to become a major threat to public health. Noise in simple terms can be defined as unwanted
or unpleasant sound which disturbs the environment and has a significant impact on the quality of
life. We all very well know how exposure to high noise level can result in hearing impairment,
headache, sleep disturbance and impaired task performance.
Noise Measurement
Three techniques are used to measure noise in the work place and community
environment
(1) Personal sound exposure meter or also known as dosimeter
(2) Sound Level Meter
(3) Tape recorders, data recorders and level recorders
Types of Noise:
Steady or Continuous Noise: It is uninterrupted noise that varies less than 5 dB-A during
the period of measurement eg. Noise from house hold fan , boiler in a power house, lathes,
diesel engine ,grinder etc
Impulsive or Impact noise: When source causes vibration for a short time eg. firing from
the gun or hammer
Intermittent/Fluctuating Noise: Large workshop number of machines are in operation, noise
levels varies from time to time or dentists drilling
Monitoring Locations
The locations for monitoring to assess the ambient noise levels shall be mix up of all
zones i.e. Residential, Commercial and Industrial to find the variations with different
zones. The monitoring schedule carried out on working days and weekend to differentiate
the noise levels between normal days to weekend days. The Sampling locations should be
sufficient enough provide representative samples for the project.
Limits in db (A)
Area code Category of area/Zone
Day Night
Time Time
(A) Industrial area 75 70
(B) Commercial area 65 55
(C) Residential area 55 45
(D) Silence zone 50 40
Table reading:
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