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Experimental Methods In Environmental Engineering: Lab. Manual
1.2. APPARATUS
Burette
Pipette
Titration flask
Measuring Cylinder
1.3. REQUIRED CHEMICALS
Auxolic Acid
Sodium hydroxide
Sulfuric acid
1.4. INDICATORS
Phenolphthalein
EBT
Solution that contains precise known concentration of substance is called a standard solution.
Normally it is expressed as moles per liter. Standards are of two types: Primary and Secondary.
A primary standard is the one which is pure, stable, high molecular weight and has no
water of hydration. Secondary standard is usually prepared in the laboratories for
specific purposes with the help of primary standards.
Molarity is defined as the ratio of the number of moles of solute and the volume of
solution (in liters), symbolized by M
Molarity-M (moles/liter) =
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Experimental Methods In Environmental Engineering: Lab. Manual
Normality is defined as the concentration equal to the gram equivalent weight per liter
of solution, symbolized by N
()
Normality-N =
()
Mass of a compound or substance that reacts with a reference compound is called gram
equivalent. It is the molecular mass of atom that reacts divided by the valence. Mass is
taken in grams. (Sawyer and McCarty 1978), (Csuros 1997)
1.6. PROCEDURE
0.1 M oxalic acid was prepared and provided. An unknown concentration of NaOH
solution was given. Firstly its molarity will be estimated using known concentration
solution of oxalic acid.
Where M = Molarity, V = volume and N = no. of moles, 1 is for oxalic acid and 2 is for
NaOH
Now calculating
(COOH)2. 2H2O + 2NaOH Na2C2O4 + 2H2O
0.110 224.3
=
1 2
Molarity of NaOH (M2) = 0.082 M
(0.10.082)100
% error as compare to 0.1 M = = 18 %
0.1
Now to standardize the sulfuric acid with the help of NaOH solution, density of
sulfuric acid is 1.84 and for it to be 0.1 M mass should be 9.8 g and using density
volume should be 5.3 mL
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Experimental Methods In Environmental Engineering: Lab. Manual
Now to react with standard NaOH 0.082 M solution with 0.1 M sulfuric acid volume is
calculated to be:
H2SO4 + 2NaOH Na2SO4 + 2H2O
33 22
=
3 2
2 is for NaOH and 3 is for Sulfuric Acid
0.13 0.08210
=
1 2
Volume of sulfuric acid used V3 = 4.1 mL
If Sulfuric acid is 0.1 M then volume used should be 4.1 mL Now to check take 10 mL of
0.082 M NaOH solution in titration flash and add indicator, color turns to pink titrate it
against sulfuric acid. Note the volume
Volume of sulfuric acid used is 5.9 mL now to find actual molarity of sulfuric acid
33 22
=
3 2
35.9 0.08210
=
1 2
Molarity of sulfuric acid (actual) M3 = 0.07 M
(0.10.07)100
% error as compare to 0.1 M = = 30 %
0.1
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Experimental Methods In Environmental Engineering: Lab. Manual
2. ALKALINIY ESTIMATION
2.1. OBJECTIVE
To estimate the alkalinity of given samples by titrating against sulfuric acid.
2.2. APPARATUS
Burette
Pipette
Titration flask
Measuring Cylinder
2.3. REAGENTS
0.02N sulfuric acid
Phenolphthalein indicator
Methyl orange indicator
Alkalinity is due to hydroxyl (OH-1), bicarbonate (HCO3-1) and carbonate (CO3-2) ions.
Alkalinity can be classified as P and M alkalinity.
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Experimental Methods In Environmental Engineering: Lab. Manual
2.6. PROCEDURE
Take 50 mL of sample in a titration flask.
Add 1ml of phenolphthalein indicator.
If Pink color doesnt appear means there is no P-alkalinity.
But if Pink color appears then P-alkalinity exists.
To find P-alkalinity titrate it against 0.02N sulfuric acid till pink color
just disappears.
Note down H2SO4 volume used, suppose P mL
Now in same solution add 1 mL of methyl orange indicator, orange color appears.
Titrate it against (0.02 N) sulfuric acid till the orange color changes to red.
Note down the volume of H2SO4 used, suppose M mL
(P(mL)N(0.02)Eq.Wt(50)1000)
Phenolphthalein alkalinity (mg/L as CaCO3) =
(Volume of sample in mL)
(M(mL)N(0.02)Eq.Wt(50)1000)
Methyl orange alkalinity (mg/L as CaCO3) =
(Volume of sample in mL)
((P+M)(mL)N(0.02)Eq.Wt(50)1000)
Total alkalinity (mg/L as CaCO3) =
(Volume of sample in mL)
1st sample:
2nd sample:
3rd sample:
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Experimental Methods In Environmental Engineering: Lab. Manual
3.2. APPARATUS
Burette
Pipette
Titration flask
Measuring cylinder
3.3. REAGENTS
Mercuric Nitrate 0.141N Hg(NO3)2
Nitric Acid
Mixed indicator (di-phenyl carbazone + Bromophenol dissolved in alcohol)
Higher concentrations of chloride in water can cause corrosion of pipes thus increasing
metal contents in the drinking water. (Sawyer and McCarty 1978), (Cohen-Adad and
Lorimer 2013)
3.5. PROCEDURE
Take 50 mL of sample in a titration flask.
Now titrate it against 0.141 N Hg (NO3)-2 mercuric nitrate till violet color reappears.
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Experimental Methods In Environmental Engineering: Lab. Manual
(A(mL)N(0.141)Eq.Wt(35.48)1000)
Cl- (mg/L) =
(Volume of sample in mL (50))
1st Sample:
Volume A used: 8.8 mL
Cl-1 (mg/L) = 880.96 mg/L
2nd Sample:
Volume A used: 7.6 mL
Cl-1 (mg/L) = 760.836 mg/L
3rd Sample:
Volume A used: 3.2 mL
Cl-1 (mg/L) = 320.352 mg/L
4th Sample:
Volume A used: 15 mL
Cl-1 (mg/L) = 1501.65 mg/L
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Experimental Methods In Environmental Engineering: Lab. Manual
4.2. APPARATUS
BOD bottles
Pipette
Burette
Titration flask
Measuring cylinder
4.3. REAGENTS
Sample
MnSO4
Alkali Azide
Conc. H2SO4
0.025 N Sodium thiosulfate Na2S2O3
Starch
Dissolved oxygen determination also plays important role in controlling the aerobic
reactions. DO also first step in calculation of biological oxygen demand. (Liptak 1994),
(Sawyer and McCarty 1978)
4.5. PROCEDURE
Take 300 mL BOD bottle and fill it completely with sample.
After that place cap on it and remove extra volume.
Add 1 mL of MnSO4 + 1mL of Alkali Azide solution.
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Experimental Methods In Environmental Engineering: Lab. Manual
If sample contains oxygen, after addition of Alkali Azide, yellow (low oxygen
intensity) or brown (high oxygen intensity) color precipitates will appear. These
precipitates are indicators of presence of oxygen. If white precipitates form, sample
contains no oxygen. If oxygen is present then proceed.
Place cap again and remove extra solution. Shake the bottle and leave it for 5-10 min
till all precipitates are settled down.
Remove the cap and add 1mL of concentrated sulfuric acid to dissolve all
precipitates. Solution color changes to reddish brown. Again, place cap on it and
remove excess solution.
Shake it and take 100 ml of it in a titration flask and titrate it against sodium
thiosulfate solution 0.025N till pale yellow color appears
Add 1 mL of starch solution. Color will change to violet.
Again titrate it against sodium thiosulfate solution till solution becomes colorless.
Note the used volume, suppose A1
Repeat the same procedure for remaining solution by taking 100 mL, 100 mL
Add these three volumes A1, A2, A3 of sodium thiosulfate to get total volume,
suppose A mL
Find DO by the given formula:
((A)(mL)N(0.025)Eq.Wt(8)1000)
DO (mg/L) =
F(Volume of sample)
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Experimental Methods In Environmental Engineering: Lab. Manual
5.2. APPARATUS
300 mL BOD bottles
Incubator
Measuring cylinder
Pipette
Beaker
titration flask
Burette
5.3. REAGENTS
MnSO4 solution
Alkali Azide solution
Concentrated sulfuric acid
0.025N Na2S2O3 solution
Reagents required for the preparation of dilution media
of two values gives BOD in mg/L. this oxygen is consumed by microorganisms present
in water to decompose the organic material present in the sample.
BOD plays a major role in water treatment processes. Low BOD means, efficient
removal of waste from water.
Before test, dilution media must be prepared very efficiently to get proper readings.
Media should be of pure distilled water with dissolved essential minerals and
adequately aerated for dissolved oxygen levels. (Liptak 1994), (Sawyer and McCarty
1978)
5.5. PROCEDURE
Take 11 BOD bottles, note their numbers and arrange them in four groups.
Three bottles in group A (A1, A2, A3),
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Experimental Methods In Environmental Engineering: Lab. Manual
mg
DO depletion ( L )300 (mL)
BOD7 (mg/l) =
volume of sample in bottle(mL)
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Experimental Methods In Environmental Engineering: Lab. Manual
After 7 Days:
Note: Since, blank sample also shows DO depletion so its effect will be included in
other sample results.
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Experimental Methods In Environmental Engineering: Lab. Manual
BOD7 :
Sample DO at zero DO at 7 days DO BOD at 7 days
added(mL) day(mg/L) (mg/L) depleted (mg/L)
(mg/L)
1 6.6 6.11 0.894 268.2
3 7.87 5.46 2.814 281.4
5 5.93 4.81 1.524 91.44
blank 7.98 7.576 0.404
After Sedimentation
At Zero Day:
Volume
of Volume
Sample
Bottle sample of DO
added
Name Na2S2O3 (mg/L)
(mL)
(mL)
(mL)
A1 1 300 9.4 6.31
A2 3 300 11.1 7.46
A3 5 300 7.7 5.21
Blank1 0 300 11.6 7.78
After 7 Days:
Volume Volume
Volume Mean
of of DO
Bottle of DO
Sample sample
name Na2S2O3
Added
(mL)
(mL) (mL) (mg/L) (mg/L)
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Experimental Methods In Environmental Engineering: Lab. Manual
Note: Since, blank sample also shows DO depletion so its effect will be included in
other sample results.
BOD7 :
BOD
DO at DO at DO at 7
Sample days
zero 7 days depleted
added(mL)
day(mg/L) (mg/L) (mg/L)
(mg/L)
1 6.31 6.07 0.66 198.47
3 7.46 5.88 2.00 199.79
5 5.21 4.44 1.19 71.32
Blank 7.78 7.36 0.42
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Experimental Methods In Environmental Engineering: Lab. Manual
5.8. APPARATUS
Reflex condenser
COD flask
Titration flask
Burette
5.9. CHEMICALS REQUIRED
K2 Cr2O7
AgCl or HgCl2
H2SO4
Ferroin solution
FAS (0.025N)
5.10. THEORETICAL BACKGROUND
The amount of dissolved oxygen in water consumed by different chemicals in it is
known as chemical oxygen demand. Sources of such chemicals are sewage, industrial
wastewater discharge, agricultural and urban runoff.
In environmental chemistry, the chemical oxygen demand (COD) test is commonly
used to indirectly measure the number of organic compounds in water. Most
applications of COD determine the amount of organic pollutants found in surface water
(e.g. lakes and rivers) or wastewater, making COD a useful measure of water quality. It
is expressed in milligrams per liter (mg/L) also referred to as ppm (parts per million),
which indicates the mass of oxygen consumed per liter of solution. A strong oxidizing
agent will produce nascent oxygen, which will combine with organic matter for
decomposition. (Sawyer and McCarty 1978), (Liptak 1994)
5.11. PROCEDURE
For COD calculation, first find COD for blank and then for your sample.
Take 50 mL of sample or mL of your choice and fill the rest with distilled water,
in COD flask and add 6-7 glass beads in it.
If the sample contains chlorides it will react with Cr2O7-2 and chlorine will be
produced, which is highly toxic. To avoid this, add a pinch of silver or mercuric
salt (nitrate). AgCl or HgCl2 will be produced. Chlorides salts of Ag or Hg are
insoluble and precipitate out hence no interference.
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Experimental Methods In Environmental Engineering: Lab. Manual
A=56
B=100
After Sedimentation
A= 75.5
B= 100
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Experimental Methods In Environmental Engineering: Lab. Manual
6.2. APPARATUS
Conical Flasks
Beaker
Spatula
Petri dishes
Filter paper
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Experimental Methods In Environmental Engineering: Lab. Manual
6.5. PROCEDURE
Prepare 10 ppm SO-24 in 100 ml.
Take 10 ml of above solution in a titration flask
Add a pinch of BaCl2 in it. White precipitates will form as it causes sulfates to
become insoluble.
Dilute it with distilled water till 100mL solution becomes.
Take Pre-weighted filter paper, suppose weight of filter paper is Wf.
Filter 10ppm sulfate solution using pre-weighted filter paper.
Transfer the filter paper in oven for dryness.
After complete drying and cooling weigh the filter paper.
Suppose this weight is WFR (filter paper + residue).
Difference will give the amount of sulfates in sample
Wf =
WFR =
Amount of sulfates =
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Experimental Methods In Environmental Engineering: Lab. Manual
References
Cohen-Adad, R. and J. W. Lorimer (2013). Alkali Metal and Ammonium Chlorides in Water and
Heavy Water (Binary Systems), Elsevier Science.
Csuros, M. (1997). Environmental Sampling and Analysis: Lab Manual, Taylor & Francis.
Udeh, P. J. (2004). A Guide to Healthy Drinking Water: All You Need to Know about the Water You
Drink, iUniverse.
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