Symbiosis Institute of Technology

Department of Applied Science (Chemistry Lab) First Year B. Tech Academic Year:
2023-24

Chemistry Practical Lab Manual

Course Outline:

Sr.No. Topics (Any 10) Hrs

1 To determine chloride ion from water sample (Mohr’s 2

methods / argentometric method)

2 To determine carbonate (CO32-), bicarbonate (HCO3-) 2

in the given water sample.
3 To determine the Total hardness (temporary + permanent 2
hardness) of water by EDTA-Na2 method

4 To determine dissolved oxygen of water sample 2

by Winkler’s method.

5 Preparation of Urea-formaldehyde (UF) resin by 2

condensation polymerization.
6 Determination of molecular weight of high polymer using 2
Ostwald’s viscometer.
7 To verify Beer-Lamberts law for solution of KMnO4 using 2
colorimeter and determine concentration in their solutions of
unknown concentration
8 To determine the moisture and ash content of the given 2
coal sample (Muffle furnace and hot air oven) Proximate analysis
9 To determine strength of acid using electrical conductivity 2
method
10 To determine the pH, TDS, TSS and Turbidity of the given 2
water sample OR cathodic and anodic coating

11 Preparation of Ni nano particles and its characterization 2

12 Determination of saponification /acid value of oil 2

13 Determination of rate constant of a reaction 2

14 To investigate the adsorption of acetic/oxalic acid by 2

activated charcoal and test the validity of Frendulich and Langmuir
isotherms
15 Potentiometry: Determination of redox potentials and Emf 2

Project work 4
Evaluation 4

Practice session 2
Recommended Pedagogy:

1. Lab Experimentation
2. Project (in case of offline mode)

Recommended Reading: Text

Books:
S. Title Author(s) Publisher details (with

No. Vol., Ed. , year, etc.)

1. Engineering Dipika Jaspal and Narosa Publisher

Chemistry:
Arti Malviya
Practical
Book
Reference Books:

1. Laboratory S.K. Bhasin & Sudha Rani Dhanpad Rai

manual on Publications
Engineering
Chemistry

Suggested Assessment/ Evaluation Methods:

A. Continuous Assessment

1. Lab Tests
B. End Semester Examination

1. Lab examination

2. Viva voce

Benchmarked against similar courses in other national/ international universities

/organizations

S. No. Title of the Course Name of University where it

is offered
1. Principles of Chemistry SRM University

2. Chemistry Savitribai Phule Pune

University
 Signature of
SR. Title of the Experiment Date Remark Subject In
charge
NO.

Determination of Chlorides from given

1 water sample by Argentometric method
[Mohr’s Method].
2-
Determination of carbonate (CO3 ),
2
-
bicarbonates (HCO3 ) from given
water sample.
Determination of total hardness of water
3
by EDTA method.
Determination of dissolved oxygen of water
4
sample by Winkler’s Method.
Preparation of Urea-formaldehyde
5
resin by condensation
To determine the molecular Weight of a high
6 polymer using its solution with different
concentrations.
To verify Beer’s law for solution of KMnO4
7 using colorimeter and
determine concentration in their solutions
of unknown concentration

To find the strength of an acid using

8
conductivity method.
To determine moisture and ash in a given
9 coal sample by proximate analysis

pH, Turbidity & TDS Measurement

10
Aim: Determination of Chlorides from given water sample by Argentometric method [Mohr’s Method].

Apparatus/reagent required:
Burette(25ml), pipette(25ml), conical flask(250ml), beaker(100ml), 0.025N Silver nitrate (AgNO3)
solution, 10% Potassium chromate(K2CrO4) indicator solution.

Theory:
Chlorides are present in water usually as NaCl , MgCl2 and CaCl2. Although chlorides are not harmful
even then their concentrations over 250ppm impart a peculiar taste to the water thus rendering the
water unacceptable for drinking purpose.

Further, existence of unusually high concentrations of chloride in a water sample indicates pollution
from domestic sewage or from industrial waste waters. Salts like MgCl2 may undergo hydrolysis
under the high pressure and temp. prevailing in the boiler, generating HCl which causes corrosion in
boiler parts. Chlorides in the form of MgCl2 and CaCl2 cause permanent hardness and are a source of
trouble not only at our house hold but also in industries.

By argentometric method chloride ions in a water sample, which is neutral or slightly alkaline can be
determined by titrating it against standard AgNO3 solution using potassium chromate as an
indicator. The pH should be between 7-8. At higher pH,
+ -
Ag +OH ⇌AgOH

And at lower pH K2CrO4 indicator is converted to K2 Cr2O7

2 K2CrO4 + 2HCl ⇌ 2KHCrO4 + K2Cr2O7 + H2O
2-
As KHCrO4 is weak in nature, concentration of CrO4 decreases and therefore, higher concentration of
+
Ag is needed for the solubility product of Ag2CrO4 to be exceeded.
 + - 2- -
Ag reacts with Cl & CrO4 when AgNO3 solution is released from the sample solution which has Cl .
+ - +
Ag + Cl ⇌ AgCl (white ppt) 2Ag
-
+ CrO4 ⇌ Ag2CrO4(red ppt)
Red colour formed because of formation of silver chromate disappears as the solution contains high
-
concentration of Cl
- 2-
Ag2CrO4 + 2Cl ⇌ 2AgCl +CrO4 .
When the concentration of chloride ions has decreased, the red colour starts disappearing slowly
and slowly on shaking and a stage is reached when all the chloride ions have formed AgCl. One extra
drop of AgNO3 at this point reacts with potassium chromate ans reddish coloured silver chromate is
formed
2AgNO3 + K2CrO4 ⇌ Ag2CrO4 + 2 KNO3

Procedure:
1) Fill burette with 0.025N AgNO3 solution up to zero mark.
2) Transfer 50ml of water sample into conical flask (using 25 ml pipette)
3) Add 8-10 drops K2CrO4 indicator solution. Yellow colored solution is obtained.
4) Slowly add 0.025N AgNO3 solution from burette and the volume of titrant is noted down as an
end point when yellow colour starts changing to brown- red.
5) Repeat the titration until the concordant volume s obtained.

Observation Table:

Volume of Burette Reading (AgNO3) ‘mL’

Sr. No.
Water Volume Constant
titrated Initial Final
Used Reading
’mL’
Calculations:

Water VS AgNO3

N1V1 = N2V2

N1 × 50 = 0.025N × V2

0.025N × V2 / 50

N1 = ……………....... N

Strength of chloride present in water sample = N1 × 35.5 ×1000 mg/L

Result table:

Strength of chloride ions in water = mg/L

 2- -
Aim: Determination of carbonate (CO3 ), bicarbonates (HCO3 ) from given water sample.

Apparatus/reagent required: Burette(25ml), pipette(25ml), conical flask(250ml), beaker(100ml),

0.02N Sulphuric acid(H2SO4), Phenolphthalein (C20H14O4) indicator solution, Methyl
orange(C14H14N3NaO3S) indicator solution.

Theory:
Presence of carbonate and bicarbonate ions constitutes the total alkalinity of water as temporary
hardness. Thus, pH of water increases to more than 7.5. This alkalinity causes corrosion, hence its
determination is also important for industrial as well as agriculture purpose.The amount of
carbonate and bicarbonate and ions present in water sample is determined by the titration with
standard sulphuric acid using phenolphthalein and methyl orange as indicators. The addition of
2-
phenolphthalein gives red colour in presence of CO3 ions and on titration with H2SO4 converts
3-
these ions to HCO ions and decolorizes the red colour.
2Na2CO3 + H2SO4 → 2NaHCO3 + Na2SO4
2- + 3-
i.e. CO3 + H → HCO
Then this colourless solution changes to yellow on addition of methyl orange. This on
titration with H2SO4 changes to rosy red coloured solution due to conversion of bicarbonate to CO2
and water.
2NaHCO3 + H2SO4 → Na2SO4 + CO2 + H2O
3- +
i.e. HCO + H → CO2 + H2O
Procedure:

1) Fill burette with 0.02N H2SO4 solution up to zero mark.

2) Pipette out 100ml (by using 25ml pipette) of the given water sample into a conical flask add 8
-10 drops of phenolphthalein indicator. The solution acquires pink
color.
3) Titrate it against standard 0.02N H2SO4 till pink colour disappears. (Color change
from pink to colorless)

4) Note down the reading as phenolphthalein end point (V).

5) Now add 8-10 drops of methyl orange in the same solution, it will give light
yellow color.

6) Continue the titration against 0.02N H2SO4 till colour changes from yellow to rosy
red.

7) Now note the extra volume of acid as V1. This is methyl orange end point.

8) The same experiment is repeated for both the sample till the concordant readings
are obtained.

Observation Table:
Burette Reading in ml

Constant
Initial Phenolphthalein end Methyl Orange end
point reading point reading reading

0.00
VP = ……ml

VM=…….ml
Calculations:

100ml of water sample upto (P) end point = ‘Vp’ml 0.02N H2SO4

100 × NP = ‘Vp’ × 0.02

NP = (‘Vp’ × 0.02)/100
NP = ‘Yp’ N

Therefore, Strength of alkalinity upto (P) end point as CaCO3

P = ‘Yp’ × 50 g/L (since, Eq. Wt. of CaCO3 = 50g/L)

P = ……. g/L
P = ……. × 1000 mg/L or ppm

Now, 100ml of water upto (M) end point = ‘VM’ ml 0.02N H2SO4

100 × NM = ‘VM’ × 0.02

NM = (‘VM’ × 0.02)/100
NM = ‘YM’ N

Therefore, Strength of alkalinity upto (M) end point as CaCO3 M = YM ×

50 g/l
M= g/l
M = ………. × 1000 mg/l
 2-
Find out relation between ‘P’ & ‘M’ from following chart & calculate the alkalinity due to CO3 &
-
HCO3

Alkalinity OH- 2- -
CO3 HCO3
(ppm (ppm)
P=0 0 0 M
P = (1/2)M 0 2P 0
P < (1/2)M 0 2P (M – 2P)
P > (1/2)M 2P-M 2(M –P) 0
P =M P=M 0 0

Therefore,
2-
Alkalinity due to CO3 = ……mg/L
-
Alkalinity due to HCO3 = ……mg/L

Result table:

A 2- ………mg/L
Alkalinity due to CO3 present in the given water sample

B - ………mg/L
Alkalinity due to HCO3 present in the given water sample
Aim: Determination of total hardness of water by EDTA method.

Apparatus &Chemicals Required:

Burette, pipette, conical flask(250ml), beaker(100ml), Measuring cylinder(10ml), 0.01M
ZnSO4 solution, Ammonical Buffer solution (pH=10) (NH3 + NH4Cl),0.01 M EDTA solution,
Eriochrome black-T indicator (EBT), etc.

Theory:
The property of water which restricts or checks the lather formation with soap is called hardness.
The soap which are sodium salts of higher fatty acids will not be forming lather till all the hardness
causing cations are lost from the water in the form of calcium and magnesium stearate , palmitate or
oleates.

EDTA Eriochrome Black-T

When Eriochrome black dye is added to the hard water at pH around 10 it gives wine red coloured
2+ 2+
unstable complex with Ca and Mg ion of the sample water. When this wine red coloured

+2 2+
complex is titrated against EDTA solution (of known strength) Ca ,Mg present in the solution

preferentially complexes with EDTA since the metal – EDTA complex is more stable than the metal –
indicator complex and liberates the free indicator at the end point thereby producing a sharp colour
2-
from wine red to blue EDTA – disodium salt of ethylenediamine tetra acetic acid. [H2y ]

+
In aqueous solution EDTA ionizes to give 2 Na ions and a strong chelating agent.

2+ 2+ 2+ 2+
Ca / Mg of water + EBT  Ca /Mg Eriochrome black –T complex

[unstable complex]
EDTA on reacting with above unstable complex forms:
2+ 2+
Ca /Mg - EDTA complex + Eriochrome black T (blue)

EBT is the metal ion indicator used in the determination of hardness by complexmetric titration with
EDTA. This dye – stuff tends to polymerize in strongly acidic solutions to a red brown product and
hence the indicator is generally used in EDTA titration with solutions having pH greater than 6.5.

2+ +
M + EBT (blue)  M-EBT (wine red) + H

2+ +
M + EDTA (pH = 10)  M – EDTA (colourless) + 2H

M – EBT (wine red) + EDTA (colourless)  M – EDTA (colourless) + EBT (blue)

The optimum pH for the determination of hardness of water is 10.0  0.1 and is adjusted by
NH4OH – NH4Cl buffer.

Procedure:
Part I: Standardization of given EDTA solution:

1) Fill burette with EDTA solution up to zero mark.

2) Pipette out 10 ml of zinc sulphate solution into a conical flask.

3) Add 2ml of Ammonical buffer solution(pH 10) and 5-6 drops of Eriochrome black – T indicator.

4) Titrate against EDTA solution taken from burette and the end point color changes
from wine red (purple) to blue color.
5) Repeat the titration until the concordant volume s obtained.

Part II: Determination of total hardness:

1) Fill burette with EDTA solution up to zero mark.

2) Pipette out 50 ml of water sample into a conical flask. Use 25 ml pipette.

3) Add 5ml of Ammonical buffer solution(pH 10) and 5-6 drops of Eriochrome black – T indicator.

4) Titrate against EDTA solution taken from burette and the end point color changes
from wine red (purple) to blue color.
5) Repeat the titration until the concordant volume s obtained.

Observations and calculations:

Part I: Standardization of given EDTA solution

Volume of Burette reading in ‘ml’

Sr.
ZnSO4 in Constant
NO. Initial reading Final reading Volume used
‘ml’ burette reading
1
2 V1 = …… ml

3
EDTA Vs ZnSO4

M1 × V1 = M2 × V2

M1 = (0.01 × 10)/ V1
M1 = ……….. M

Therefore, Exact Morality of EDTA solution (Mex) =… M

Part II: Determination of Total hardness of water.

Volume of Burette reading in ‘ml’

Sr. water
NO. sample in Initial Final reading Volume used Constant burette
‘ml’ reading reading

1
2 V3 = …… ml

Water sample Vs EDTA

M4 = Mex × V3
x 100
M = (Mex × V3)/ 100
4
M = ……….. M
4
Molarity of Tap water × Molecular
Weight of calcium carbonate =
per liter weight of CaCO3
= M4 × 100.071× 1000mg/L
= ________ g/L

Result Table:

1. Exact Molarity of EDTA solution ……………. M

2. Total hardness of the given water sample ……………. mg/L

Aim: Determination of dissolved oxygen of water sample by Winkler’s Method.

Apparatus & Reagent required:

Burette (25 ml), pipette (25ml), conical flask (250ml), Stoppered bottle(250ml), 0.01N Sodium
thiosuphate(Na2S2O3)solution, Manganous sulphate(MnSO4 ) solution, Alkaline iodide(KI)
solution, starch indicator and Conc.HCl.

Theory:
The level of dissolved oxygen depends on the physical and chemical activities of water body. The
analysis of D.O. plays a key role in water treatment, process control and water pollution control
activities.
Winkler’s method is based on the fact that dissolved oxygen oxidizes KI toiodine. The
liberated iodine is titrated against standard sodium thiosulphate (also known as hypo) solution
using starch as an indicator. Since dissolved oxygen in water is in molecular state, it cannot oxidize
KI. Hence manganese hydroxide is used as an oxygen carrier to bring about the reaction between KI
and oxygen. Manganese hydroxide in turn is obtained by the reaction between KI and oxygen.
-
The oxidizing agents present in water like nitrites and ferric ions oxidize I to I2 and give a positive
error. Hence sodium azide is used in alkaline iodide solution to decompose these.

Reactions:
MnSO4 + 2KOH → Mn(OH)2 + K2SO4

Mn(OH)2 + O2 → 2 MnO(OH)2

MnO(OH)2 + H2SO4 → MnSO4 + H2O + [O]

2KI + H2SO4 + [O] → K2SO4 + H2O + I2 ↑

2Na2S2O3 +I2 → Na2S4O6 + 2NaI
Procedure:
1) Fill burette with 0.01N Sodium thiosuphate solution up to zero mark.
2) Take 100 ml water sample in to the Stoppered bottle and add 2 ml Manganous
sulphate (MnSO4) solution and 2 ml Alkaline iodide(KI) solution from common burette.
3) Shake thoroughly, wait for precipitate to settle.
4) Immediately Add Conc. HCl and 8-10 drops of starch indicator close the bottle &
shake well. Black-Blue color will appeared.
5) Titrate this against 0.01N Sodium thiosuphate solution. End point is indicated by
Black-Blue color to colorless.
6) Repeat the titration until the concordant volume s obtained.

Observations:

Burette Reading in ‘ml’

Sr.No. Volume of Water
titrated ’ml’ Volume Concordant
Initial Final
Used Reading

Calculations:
Water Vs Na2S2O3

N1 × V1 = N2 × V2

(0.01 × V2 )/ 100
N1 × 100 =

N1 = ……….. N

Therefore, Strength of oxygen = N1 × 8 g/L (equivalent weight of oxygen O2=8)

Result:
1. Dissolved oxygen in 100 mL of water sample =… g/L
Aim: Preparation of Urea-formaldehyde resin by condensation.

Apparatus & Reagents required: Beaker(100ml), Glass rod, watch glass, Formaldehyde solution, Urea
and Conc. H2SO4.

Theory: Phenolic resins are condensation polymerization of phenolic derivatives with aldehydes.
Urea-formaldehyde resin is prepared by the condensation reaction with urea and neutral or alkaline
conditions. Such resins find uses in packaging, accessories, and unbreakable dishes water.

Reaction:
Procedure:

1) Weight the 3 g of urea on weighing paper at weight balance

2) Weight the empty watch-glass & note down the weight.

3) Take 5 ml of formaldehyde solution in to the 100 ml Beaker.

4) Add little-little quantity of urea in to the formaldehyde and stir it by using glass
rod. Dissolve the whole 3 gm of urea in to the formaldehyde.

5) Put whole solution on watch glass and add dropwise Conc. H2SO4 solution.

6) After 5-10 minute the white resin is form, wash this under running water to
remove excess material and only white resin is stick to the watch-glass.

7) By using tissue paper remove the water and make it dry.

8) After removing water droplets, take the weight of watch-glass and note down the
same.

9) Watch-glass as it is submit to Instructor.

Weight of polymer is gm.

Aim: To determine the molecular Weight of a high polymer using its solution
with different concentrations.

Apparatus: Ostwald’s viscometer, Stop watch, pipette.

Chemicals: Pure solvent (Distilled water), 0.5, 0.4, 0.3, 0.2, 0.1% solutions of unknown
polymer, distilled water.

Theory:
Polymers have molecular weights, which may vary from several thousands to several millions. It is
related to the chain length and the extent of cross-linking between different chains.
Addition of even a very small amount of a polymer to a low viscosity solution causes a sharp
increase in its viscosity. The magnitude of increase in viscosity depends on the molecular weight of
the polymer.When a liquid is made to flow through a capillary tube by a pressure gradient and the
time for a given volume to flow along the tube is measured, then at a constant temp., the coefficient
of viscosity (η), is given by the Poiseuille’s equation,

4
η = (π P r t) / (8 V L)
Where, V-volume of liquid that flows through the tube
P- Difference in pressure at the two ends of the tube. r-
Radius of the tube.
L- Length of the capillary tube in centimeter. t-
Time of flow in seconds.

When viscometer is used for the measurement of the liquid flows vertically down the
capillary tube and the driving force is given by,
P = hpg
By using an Ostwald’s viscometer, relative viscosity ηr = η/ η0 can be found out. Here is the
viscosity of the polymer solution and η0 is the viscosity of pure solvent.
ηr = ηs / η0 = Ps ts / P0 t0
Ps and P0 are densities of unknown liquid (polymer solution) and pure solvent respectively ts and t0
are the corresponding flow times.
For a dilute polymer solution (C < 0.5% ), the density of the solution may be taken as that of the
solvent, i.e. Ps = P0
ηr = ts /t0
The specific viscosity, ηsp= (ηsp - η0)/ η0 = ηr - 1
The ratio of the specific viscosity of the solution to its conc. C, expressed in g/100ml is called
reduced specific viscosity or simply reduced viscosity ηred
ηred = ηsp / C
Both and vary sharply with conc., the variations with conc. is somewhat less and regular, and the
plot of versus conc. is a straight line given by the equation. The value of the constant is given by the
intercept on the ordinate.
This constant, which becomes independent of concentration is the limiting value of the reduced
viscosity and is termed as limiting viscosity or intrinsic viscosity [η]
Mathematically,

Lim ηred / C or ηsp / C = mC + [η]

[η]=C→0

For linear polymer the intrinsic viscosity (η) and the molecular weight M are generally found
to obey the Mark-Kuhn- Houwink empirical equation.
Where K and α are constants for a particular polymer/ solvent/temperature system. K and
α, values are known for a polymer/solvent combination, M may be calculated from the determined
value of [η].
0
The values of K and α are given below for some polymer (25 C)

Procedure: Perform the experiment in two parts

Part I: To determine the time of flow for a given pure solvent.

1. Take a clean and dry viscometer.
2. Introduce exactly 10ml of pure solvent (e.g. distilled water) to the viscometer from the
clamp side.
3. Suck the liquid from capillary side by means of rubber tube, above the mark ‘x’.
4. Release the liquid and start stopwatch when liquid leaves upper mark ’x’.
5. Stop the stop-watch when liquid reaches lower mark ’y’.
6. Take three time of flow ( in seconds) for a liquid flowing from ‘x’ to ‘y’.
7. Record three readings. Remove the pure solvent from the viscometer.
 Part II: To determine the time of flow for given solution of polymer.
1. Introduce exactly 10 ml of the 0.1% solution of unknown polymer in to the
viscometer from clamp side.
2. Repeat the procedure from (4) to (6) as given in part I.
3. Record the time of flow (in second) for 0.1% solution of polymer.
4. Similarly repeat the procedure for 0.2, 0.3, 0.4, 0.5% solution of polymer and record the
time of flow.

Observation Table (Part

I):

Solvent Time of flow (in sec) Mean Time to(in sec)

1 2
Distilled Water

(Part II):

Flow Time
Concentration t/t0 = η/η0 η sp= η/η0-1 η sp/%C
1 2 Mean

0.1%

0.2%

0.3%

0.4%

0.5%

Graph :
[η] = α
KM

Mα = [η]/K
α log M = log [η] – log K
log M = { log [η] – log K}/ α
M = …………
Calculation
Result: The molecular weight of the polymer is ………
Aim:

To verify Beer’s law for solution of KMnO4 using colorimeter and determine concentration in their
solutions of unknown concentration.

Apparatus/reagent required:
Digital Colorimeter, Cuvette, Beaker(100 ml), Test tubes (10ml), 0.001M KMnO4 and Distilled water.

Theory:
1. Lambert’s law: When a beam of monochromatic light is allowed to pass through a transparent
medium, the rate of decrease of radiant power with the thickness of the medium is directly
proportional to the radiant power of the incident light.
Mathematically,
-(dP/db)  P or -(dP/db) = k1P

On integrating the above equation between limits b=0 and b=b and P=P0 and P=P,We get,
-k1x
(P/P0) = e here, (P/P0) = T = transmittance of solution.

Or log10(P0/P) = [k1/2.303]b, here, log10(P0/P) = A = absorbance of solution.

Therefore, A = K1b where k1 = (k1/2.303)

i.e. absorbance of the solution is directly proportional to the path length of the solution.

2. Beer’s law: When a beam of monochromatic light is allowed to pass through transparent
medium, the rate of decrease of radiant power with the concentration of the medium is directly
proportional to the radiant power of the incident light.
Mathematically, the law may be stated as follows:
-(dP/dC)  P or -(dP/dC) = k2C
On integrating the equation between limits P=P0 and P=P and C=0 and C=C, we get,

-K2C
(P/P0) = e here, P/P0 = T = transmittance of solution.
Or log10 (P/P0) = [k2/2.303] C here, log10 (P/P0) = A = absorbance of solution.
Therefore, A = K2C where K2 = [k2/2.303]

i.e. absorbance of the solution is directly proportional to the concentration of the solution.
3. Lambert- Beer’s law:

The lambert’s law states that,

Absorbance = Constant × thickness of the medium (b)

The Beer’s law states that,
Absorbance = constant × concentration of the medium(c)
The combined law (Beers lamberts law) may be given the relation,

Absorbance (A) = constant x b x c

Procedure:
For determination of ʎmax :
1) Take out 5 test tubes.
2) And fill this test tube as per following:
Test Tube Number 0.001 M KMnO4 Distilled Water
1 2 ml 8 ml
2 4 ml 6 ml
3 6 ml 4 ml
4 8 ml 2 ml
5 10 ml 0 ml
3) Take around 1 ml least diluted KMnO4 solution in one of the cuvette. And around
1 ml distilledwater in to another cuvette. Wipe out the outer surface of both the cuvettes by using
tissue paper.

4) Set the filter at 400nm and put the cuvette which contains distilled water in the sample
compartment. Make the zero set by using knob.
5) Replace the distilled water cuvette by cuvette contains KMnO4 solution. And note the absorbance
at that particular wavelength.
6) Repeat the process for each wavelength.
7) Plot the graph of “Wavelength” Vs “Absorbance”. The wavelength at which
absorbance is maximum is known as ʎmax .
For determination of unknown concentration:
1) Put the ʎmax filter in the instrument & set the zero using distilled water.
2) Note the absorbance value of each concentration at that wavelength(ʎmax)
3) Also take the reading for unknown concentration.
4) Plot the graph of “concentration” Vs “Absorbance”.
5) By drawing dotted line, show the unknown concentration.

Observation table:

1) λmax determination:

Absorbance / Optical
Sr. NO. Wavelength (λ in nm)
density
1
2
3
4
5
6
7
 2) Unknown concentration determination:

Sr. Concentration (C) in Optical density

No. moles/lit (O.D.) (A)
1
2
3
4
5
6 Unknown

Plot the graphs as: (i) Wavelength against Absorbance

(ii) Concentration against Absorbance

By knowing the absorbance of unknown solution, the corresponding concentration value can be
determined graphically.

Calculations:

Results:
1. The ʎmax for KMnO4 is =……………..
2. The unknown concentration has been found to be =… M
Aim: To find the strength of an acid using conductivity method.

Materials Required: NaOH, HCl, conductivitimeter, beaker(250 ml), and burette(25 ml)

Theory:
The experiment helps to determine the point where reaction is completed using a conductometer.
This instrument measures the changes in conductance of solution, produced by the ions in the
solution. It works on the principle of ohm’s law.
The acid whose strength is to be determined is taken in a beaker and the electrode of
conductometer is dipped into the acid solution. This measures the conductance of acid. Now this acid
solution is titrated against the base of known molarity where the conductance starts decreasing. This
is due to the binding of H+ ions of acid with the OH- of Base until a point is reached where
conductance is minimum. When we move forward the conductance starts increasing again. This is
now due to the free ions of base present in solution.
This point at which this transition occurs is called Equivalence point. At Equivalence point we
measure the volume of base used to neutralize the acid ions completely in the solution. Using these
values, the strength of acid can be calculated.
The conductance of the solution mainly depends on two factors
1. Size of the ions
The conductivity of the solution is inversely proportional to the size of the ions. If the size of the ions
is increasing, then the conductivity of the solution will decrease because the mobility of the ions will
decrease by increasing the size of the ions.
 Initially solution contain the hydrogen ions when this solution is titrated against the base
solution, the base reacts with the acid and the number of the hydrogen ions go on decreasing. Finally,
a stage reaches when there is no hydrogen ion in the solution so the conductivity decreased and
remains constant. If further base is added, then the number of negative ions increases and the
conductivity go on increasing. The point at which the conductivity becomes constant is the
equivalence point. The volume of base used at equivalence point is used to calculate the molarity of
acid and then the strengthof acid.
In solution of a strong acid, hydrochloric acid, HCl for instance, to which a solution of a strong
base, sodium hydroxide NaOH, is added. The reaction occurs. For each amount of NaOH added
equivalent amount of hydrogen ions is removed. Effectively, the faster moving H+ cation is replaced
by the slower moving Na+ ion, and the conductivity of the titrated solution as well as the measured
conductance of the cell fall. This continues until the equivalence point is reached, at which we have a
solution of sodium chloride, NaCl. If more base is added an increase in conductivity or conductance is
observed, since more ions are being added and the neutralization reaction no longer removes an
appreciable number any of them. Consequently, in the titration of a strong acid with a strong base,
the conductance has a minimum at the equivalence point. This minimum can be used instead of an
indicator dye to determinethe endpoint of the titration. Conductometric titration curve that is a
plotof the measured conductance or conductivity values against the number of milliliters of NaOH
solution

2. Temperature:
By increasing the temperature, the mobility of the ions in the solution will increase. So temperature
has a direct effect on conductance of solution. E.g. by increasing the temperature the conductance
will increase and vice versa.

Procedure:
1) Fill burette with 0.1 NaOH Solution.
2) Take 100 ml give acid (HCL) solution in to the Beaker (250ml).
3) Calibrate the conductivity-meter as per following:
i) Put the conductivity cell in to the distilled water.
0
ii) Set the temperature 25 C in the instrument.
 iii) Adjust the cell constant 0.98 using knob.
iv) Put knob on conductance. Machine is ready to take the reading.
4) Remove the conductivity cell from distilled water and put in to the acid (HCL)
solution.
5) Slowly shake and note down the stable reading.
6) Add 1ml of NaOH solution from the burette and slowly shake, note the stable
reading. Note down the reading at each addition of 1 ml NaOH similarly.
7) Plot the graph of “ Vol of NaOH added” Vs “ Conductance”
8) Peak value use as the end point of titration.

Observations:
Sr. NO Volume of Base used (mL) Conductance
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
Calculations:
Acid Base
M1V1=M2V2

M1= M2V2 = M1V1

V1 100
Strength of acid = Molarity (M1) x Molecular Wt.

=M1 x 36.5(For HCl)

= g/ml

Result: Therefore strength of the acid using conductivity method is ---------

Aim: To determine moisture, volatile and ash in a given coal sample by proximate analysis.

Apparatus & chemicals required:

Coal sample, Silica and Porcelain crucible, long legged tongs, heating instruments like Muffle furnace and
oven etc.

Theory:

Moisture:
Free water may exist in the coal as adsorbed on the surface, condensed inside fine capillary
network and as bound to the coal molecule by chemisorption and hydrogen bonding.

Ash:
Coals are associated with certain mineral or inorganic matter, which gets deposited along with
vegetable matter or gets into coal by subsequent infiltration. The ash consists mainly of silica,
alumina, iron oxide and lime. When heated, coal as does not melt sharply at any temperature, but
begins to soften at much lower temperature than that required melting. The ash content in coke is
much higher than in coal.

Procedure:

For Moisture content:

1) Take porcelain crucible note down its identification number and empty weight at
weighing balance.
2) Put 1gm coal sample into the crucible carefully.
3) 0
Put the crucible into Hot Air Oven by using tong. ( Temperature : 110 C)
4) Remove the crucible after 30 minute, cool down for 5 min & take the weight.

For Ash Content:

1) Take silica crucible note down its identification number and empty weight at
weighing balance.
2) Put 1gm coal sample into the crucible carefully.
3) 0
Put the crucible into Muffle furnace by using tong. ( Temperature : 750 C)
4) Remove the crucible after 30 minute, cool down for 15 min & take the weight.
Observations & calculation: For
Moisture content:
Sr. NO Description Value
1 Weight of empty crucible (X) Xg =
2 Weight of crucible + coal sample (Y) Yg =
3 Weight of crucible + sample, after heating (Z) Zg=

% of moisture = [ (Y-Z) / (Y-X) ] x 100

For Ash Content:

Sr. NO Description Value
1 Weight of empty crucible(X’) X’ g =
2 Weight of crucible + coal sample(Y’) Y’ g =
3 Weight of crucible + sample, after heating(Z’) Z’ g =

% of Ash = [(Z’- X’) / (Y’- X’)] ×100

Result Table:

1 Percentage of moisture =

2 Percentage of ash =
 TDS, pH & Turbidity

Aim : To determine the Total Dissolved solids (TDS), pH & Turbidity of the given water sample.

TDS Measurements

Requirement: TDS meter, Standard solution, 250mL beaker, water sample.

Theory:

Total suspended solids (TSS) and Total dissolved solids (TDS) measure the amount of particulate
matter (tiny pieces of things) floating in water. In lakes and rivers, this can include particles from
algae, other organic matter, silt and clay, and other inorganic
substances (such as minerals, salts and metals).
These particles, or ‘solids’, can be divided into two types by
passing the water through a filter. The particles that are large
enough to be held back by the filter are called total suspended
solids (TSS), while the particles that pass through the filter are
called total dissolved solids (TDS).

Total suspended solids (TSS) values are often related to the turbidity (cloudiness) of water. If TSS is
high and the water is murky then light from the sun will not travel well through the water, making it
difficult for plants and algae to grow. This, in turn, can reduce productivity (the amount of plant and
animal life that a river or lake can support) and oxygen generation. Lot of soil and silt in the water can
also clog fish gills and, if it settles to the bottom, bury fish eggs. Total dissolved solids (TDS) include
dissolved minerals and salts in the water. As a result, TDS is often closely related to conductivity,
salinity, alkalinity, and hardness measures. Most freshwater fish and bugs cannot tolerate high TDS
because they are not adapted to saline (salty) water, like marine fish are.

Procedure:

0
1) Put the cell in distilled water and set the temperature 25 C in the machine.

2) Now dip the cell in standard solution and calibrate the TDS as 0.9185ppt (parts per trillions)

3) Dip the cell in distilled water and wipe it out and then dip into the water sample.

4) The reading shows the TDS present in the given water sample.

pH Measurements
Requirement: pH meter, standard solution, 250mL beaker, water sample.

Theory:
pH of water is a measure of amount of hydrogen ions that is present in the water. It determines if
the water is alkaline or acidic in nature. pH stands for potency of hydrogen ions. As per the World
Health Organization (WHO), value of pH for the water is 6.5 to 8.5. pH can be calculated
mathematically as:
pH = -log [H]
This scale was developed by the scientist Sorenson in the year 1909. The below reaction implies that the
water shows that the number of H+ and OH- ions are equal in amount experimentally. It has also been
proved that the product of both the concentration is equal to a constant ‘K’. The value of this constant
found to be between 10 and 14.
+ -
H2O → H + OH

For acids, the pH value is between 1 to 7, and for bases from 7 to 14.
Procedure:

0
1) Put the cell in distilled water and set the temperature 25 C in the machine.

2) Now dip the cell in standard solution and calibrate the pH as 4, 7 and 9.2

3) Dip the cell in distilled water and wipe it out and then dip into the water sample.

4) The reading shows the pH of given water sample.

Turbidity meter/Nephelometry
Requirement: Turbidity meter, standard solution, turbidity sample bottle, water sample.

Theory:
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.

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 for water treatment. 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.
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 higher the intensity of scattered
light the higher is the turbidity. Formazin polymer is used as the primary standard reference
suspension. Procedure:

1) Put the distilled water bottle in sample slit and set the zero.

2) Now remove the distilled water and insert the standard bottle and set the reading as
100 NTU

3) Remove the standard and insert the sample.

Observation and Result:

The ........, ……….. and of the water samples have been observed.