APPLIED CHEMISTRY LABORATORY MANUAL

CY19143

COMMON TO I SEM. B.E. – EEE & CSE AND B.TECH.-IT

AND II SEM. B.E. - CIVIL

ACADEMIC YEAR 2020 –2021

NAME : ––––––––––––––––––––––––––––

ROLL NO. : ––––––––––––––––––––––––––––

BRANCH : ––––––––––––––––––––––––––––

DEPARTMENT OF HUMANITIES & SCIENCES –CHEMISTRY

RAJALAKSHMI ENGINEERING COLLEGE

THANDALAM-602 105

1
 CONTENTS
S.No. Experiment Page
No.
1 Estimation of mixture of acids by conductometry 3
2 Estimation of extent of corrosion of iron pieces by
6
potentiometry
3 Estimation of the extent of dissolution of copper / ferrous ions
9
by spectrophotometry
4 Estimation of acid by pH metry 11
5 Determination of total, temporary and permanent hardness by
13
EDTA method
6 Estimation of DO by winkler’s method 17
7 Estimation of alkalinity by indicator method 20
8 Estimation of chloride by argentometric method 24
9 Estimation of sodium and potassium in water by flame
27
photometry
10 Determination of flash and fire point of lubricating oil 31
11 Determination of cloud and pour point of lubricating oil 33
12 Determination of corrosion rate on mild steel by weight loss
34
method
13 Determination of molecular weight of a polymer by viscometry
36
method.
14 Adsorption of acetic acid by charcoal 40
15 Determination of phase change temperature of a solid 42

2
 CONDUCTOMETRIC TITRATION OF MIXTURE OF ACIDS

Exp. No. 1 Date:

AIM
To determine the strength and amounts of strong acid (SA) and weak acid (WA)
present in the given acid mixture. A Standard solution of NaOH of strength ….. N is
provided.

PRINCIPLE
Solution of electrolytes conducts electricity due to the presence of ions. Since
Specific conductance of a solution is proportional to the concentration of ions in it,
conductance of the solution is measured continuously during the titration, to find the end
point.

HCl + NaOH NaCl + H2O (I neutralization)

CH3COOH + NaOH CH3COONa + H2O (II neutralization)

For example , when a mixture of HCl and CH3COOH is titrated with NaOH the fast
moving hydrogen ions are progressively replaced by slow moving sodium ions to form
salt and water. As a result, conductance of the solution decreases. This decrease will
take place until the HCl neutralisation point is reached.
Further addition of alkali results in formation of sodium acetate. Since sodium
acetate is a stronger electrolyte than acetic acid, conductance slowly increases until all
acetic acid is completely neutralized(II-Neutralisation). Furthermore addition of alkali
increases the conductance sharply due to the addition of fast moving OH- ions.

PROCEDURE
Fill up the burette with NaOH solution up to zero mark. Make up the given
unknown solution (mixture of a weak & a strong acid) to 100ml in a standard flask with
distilled water. Pipette out exactly 20ml of the made up solution into a clean 100ml
beaker and dilute it to 50ml using distilled water. Introduce a conductivity cell into the
solution and connect the terminals to a conductivity meter.
Add NaOH from the burette to the Acid mixture in the beaker in terms of 0.5ml
increments. Stir the solution using a glass rod, and observe the conductance values for
every addition. Continue the titration after the endpoint, for a minimum of 3ml of the
burette solution. The conductance values decrease initially, then gradually increase and
finally show a steep increase. The titration hence shows two endpoints (ie) I
neutralization for (strong acid) & II neutralization for (weak acid).

Calculate the strength and amount of the acids using the endpoints obtained from the
graph.

3
 SHORT PROCEDURE
Estimation of SA and WA
CONTENTS
Std. NaOH Vs SA+WA MODELGRAPH
Burette solution Std. NaOH
Pipette solution 20ml acid mixture (SA+WA)
Additional solution 30ml distilled water
Electrode/Cell used Conductivity cell
Instrument used Digital Conductivity meter

1.Decrease to increase of conductance

End point 2. slow to rapid increase of
conductance

Std. NaOH Vs Strong acid

Volume of NaOH Observed conductance
S.No.
added (ml) (10-3 mho or m mho)
1.

1
2.

2
3.

3
4.
5.
6.
7.
8.
9.
10.

11.

12.

13.

14.

15.

16.

17.

18.
4
 19.

20.

21.
(i) Calculation of
22.
strength of Strong Acid
Volume of NaOH (V1) = ---
23.
------ (a)ml (from graph)
Strength of NaOH (N1) = ---
24.
------ N
Volume of HCl (V2) = 20
25. ml
Strength of HCl (N2) = ---
26. ------?
N2 =
27. (V1 × N1 ) / V2
Strength of HCl = ---
28. ------- N
Amount of HCl present in the
29. solution = Strength of
HCl×36.5(eq.wt of HCl)
30. =---------- g/l.
(ii) Calculation of strength of
Weak Acid
Volume of NaOH (V1) = ---------(b-a)ml (from graph)
Strength of NaOH (N1) =---------N
Volume of CH3COOH (V2) = 20 ml
Strength of CH3COOH (N2) = ---------?
N2 = (V1 × N1 ) / V2
Strength of CH3COOH = ---------- N
Amount of CH3COOH present in the solution =
Strength of CH3COOH ×60 (eq.wt of CH3COOH)
=--------- g/l.

RESULT
(i) The strength of acids present in the given unknown solution are
a) Strong acid =---------- N b) Weak acid = ---------- N
(ii) The amount of Strong acid present in the given solution = ---------- g/l
(iii)The amount of Weak acid present in the given solution = ---------- g/l

5
 ESTIMATION OF EXTENT OF CORROSION OF IRON SPECIMEN BY
POTENTIOMETRY
Exp. No. 2 Date:

AIM
To estimate the amount of extent of corrosion by estimating the ferrous ions present in
the whole of the given solution by potentiometric titration using standard decinormal
potassium dichromate.

PRINCIPLE
Potentiometric titrations depend on measurement of emf between reference
electrode and an indicator electrode. When a solution of ferrous ion is titrated with
acidified potassium dichromate solution, the following redox reaction takes place.
6Fe2+ + Cr2O72- + 14 H+ 6Fe3+ + 2Cr3+ + 7H2O
During this titration, Fe2+ is oxidised to Fe3+ and its concentration increases. At the end
point, there will be a sharp rise in the emf value. This is called “Sweeping potential”. It
indicates complete formation of Fe3+ ions at the end of redox reaction.

The cell is set up by connecting this Fe2+/Fe3 redox electrode with a calomel electrode as
shown below:
Pt, Fe2+, Fe3+ // KCl , HgCl2 (s), Hg
A graph is drawn between emf measured against the volume of potassium
dichromate added. The end point is noted from the graph.

PROCEDURE
Pipette Solution
Iron pieces are taken and washed thoroughly and immersed in conc. Sulphuric acid
overnight. This is then made upto 100 mL.

6
 Transfer the given Ferrous solution into a 100ml standard flask and make it upto the mark
using distilled water. Fill in standard potassium dichromate solution into the burette
upto the mark.
Pipette out 20ml of Ferrous solution into a 100ml clean beaker. Add 10ml of dil.
H2SO4 and 20ml of distilled water to it. Dip in a platinum electrode and a calomel
electrode into this solution and connect to a potentiometer. Then add Potassium
dichromate interms of 0.5ml/addition from the burette to the solution in the beaker and
stir it well. For each addition of the solution from the burette note the emf of the cell
using the potentiometer. Continue the titration atleast six reading after the “Sweeping
potential”.
Plot a first derivative graph by taking ΔE/ΔV versus volume of K2Cr2O7.The
strength of ferrous solution and the amount of ferrous ion present are calculated from the
end point.

SHORT PROCEDURE
Estimation of Iron
CONTENTS MODELGRAPH
Std. K2Cr2O7 Vs Fe2+
Burette solution Std. Potassium dichromate
Pipette solution 20ml Ferrous ion soluion
10ml dil.H2SO4 and20ml
Additional solution
distilled water
Platinum-Indicator electrode
Electrodes
Calomel-20 reference electrode
Instrument used Digital potentiometer
Sudden/rapid increase in emf
End point
Value

Std K2Cr2O7 Vs FeSO4

Volume of Potassium Emf ∆V in ∆E/∆V in
S.No ∆E in mV
Dichromate in ml 10-3 Volt ml mV/ml
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.

11.

7
 13.

14.

15.

16.

17.

18.

19.

20.

21.

22.

23.

24.

25.

26.

27.

28.

29.

30.

CALCULATION:
Volume of Potassim dichromate (V1) = ---------- ml (from graph)
Strength of Potassium dichromate (N1) = ---------- N
Volume of Ferrous sulphate (V2) = ---------- ml
Strength of Ferrous sulphate (N2) = (V1 × N1 ) / V2

8
 = ------------ N
Amount of Ferrous ion present = Strength of ferrous × Equivalent wt
in 1000ml of the solution solution of Fe (55.85)

= ………… g
RESULT
The amount of Ferrous ion present in the given solution is = ------------ g/l.

ESTIMATION OF THE EXTENT OF DISSOLUTION OF FERROUS IONS

BY SPECTROPHOTMETRY
Exp. No. 3 Date:
AIM
To determine the amount of iron dissolved in the given sample by spectrophotometry

9
PRINCIPLE
When a monochromatic light passes through a homogeneous coloured solution, a portion
of incident light is reflected, a portion is absorbed and the remaining is transmitted.
Io = Ir + Ia + It
Where, Io , Ir = intensity of light entering solution and Intensity of light
reflected
Ia , It = intensity of light absorbed and Intensity of light transmitted

Ir is usually eliminated and hence Io = It + Ia . The mathematical statement of Lambert

– Beer’s law is given by
T = I / Io = 10 -Cl (or) A = log Io / I = Cl
Where T = transmittance of solution
I = intensity of light leaving solution (transmitted light)
 = molar absorption co-efficient
c = concentration of the solution in moles/litre
l = Path length of light through the solution in cm
A = absorbance or optical density of the solution.
When a ray of monochromatic light passes through an absorbing medium, its intensity
decreases exponentially as the concentration of the absorbing substance and the path
length. Keeping the path length constant, say l=1 cm, the variation in absorbance is with
respect to only concentration, C.
Fe3+ ions in low concentrations does not give any colour in solution. However, it
develops a red colour when it reacts with KCNS solution.
Fe3+ + 6KCNS  [Fe (CNS) ]3- + 6K+
Red coloured complex

Further, this colour is in the blue region, ( = 480 nm). Spectrophotometer has a wide
range of adaptability that allows selection of monochromatic light of any wavelength in
the visible spectrum. Therefore spectrophotometry is used to find very low concentrations
of Fe3+ ion solutions.

LAYOUT OF SPECTROPHOTOMETER

10
PROCEDURE
Preparation of Ferrous ammonium sulphate (standard solution)
From stock solution given 1 mL, 2 mL, 3 mL, 4 mL, 5 mL, 6 mL is pipetted out in
different 100 mL standard measuring flasks. 1-2 drops of 0.1 N potassium permanganate
(until a slight pink colour is seen) and the 2-4 mL of 20% potassium thiocyanate (KCNS)
is added and made upto 100 mL.
Preparation of unknown solution
50 mL of the given sample is taken in 100 mL standard measuring flask. This is acidified
with 1:1 HCl, and one drop of 0.1N Potassium permanganate and 2-4 drops of 20%
potassium thiocyanate (KCNS) are added. It is made upto 100 mL (i.e. if the value is out
of range it is diluted).The spectrophotometer is switched on and is allowed to warm up
for ten minutes. The monochromator is adjusted for wavelength 480 nm. The blank
sample is kept in the cell and light transmission is adjusted to 100 (or absorbance to
zero). The standard solutions of known concentrations that are already prepared are kept
in the sample holder one by one and the corresponding absorbance is noted. Similarly the
OD/absorbance is noted for unknown solution.

SHORT PROCEDURE
MATERIAL / SOLUTION/
CONTENTS
TREND MODELGRAPH
Cuvette Solution Ferrous solution
Potassium permanganate &
Additional solution
Potassium thiocyanate
Instrument used Spectrophotometer
The absorbance values of every ppm
End point
of ferrous solution are noted

Determination of Absorbance

11
 S.No Vol. of Vol. of Vol. of Vol. of Concn Absorbance
Stock dil.HNO3 1% distilled of Fe2+ ions
soln. (ml) NH4SC water (ppm)/N
N
(ml)
1
2
3
4
5
6

RESULT
The amount of iron present in the given solution = ………. ppm

ESTIMATION OF ACID BY pH METRY

12
Exp. No. 4 Date:
AIM
To determine the strength and amount of given HCl by pH metry. A standard
solution of --------N NaOH is provided.

PRINCIPLE
The pH of a solution is related to H+ ions concentration by the following formula.
pH = -log 10 [ H+ ]
When NaOH is added slowly to HCl, H+ ions get neutralized by OH- ions. The
pH increases slowly.
H+ + Cl- + Na+ + OH- Na+ + Cl- + H2O
When all H ions of HCl are neutralized at the end point, addition of NaOH causes
+

high increase in pH because of the excess OH- ions.

PROCEDURE
Fill the given Standard Sodium hydroxide solution in a clean burette. Transfer the
given solution of HCl carefully into a 100ml std.flask and make it up to the mark using
distilled water. Now pipette out 20 ml of the HCl solution into a clean beaker. Then
dilute it to 50ml with distilled water. Dip a glass electrode into the solution and connect
to a pH meter.

Now add NaOH gradually from the burette to HCl solution taken in the beaker.
Note the pH of the solution for each addition of NaOH. Continue the titration until at
least 5 readings after the endpoint. Plot a graph between ΔpH/ΔV and the volume of
Sodium hydroxide.
Draw a graph as depicted in the diagram. The volume corresponding to the peak
ΔpH/ΔV is the sharp Equivalence Point and it is equal to the volume of NaOH exactly
required for neutralization of the strong acid.

13
SHORT PROCEDURE
Estimation of Acid
CONTENTS MODELGRAPH
Std. NaOH Vs Acid
Burette solution Std. NaOH
Pipette solution 20ml Acid
Additional solution 30ml distilled water
Ion selective electrode/pH
Electrode/Cell used
electrode/combined electrode
Instrument used Digital pH meter
Sudden/rapid increase in pH
End point
value
Std.NaOH Vs HCl
S.No Volume of pH ∆pH ∆V ∆pH/∆V
NaOH (ml)
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.

14
Calculation:

Volume of NaOH (V1) = ----------- ml (from fair graph)

Strength of NaOH (N1) = ----------- N
Volume of HCl (V2) = 20 ml
Strength of HCl (N2) = (V1 × N1 ) / V2

Strength of HCl = ---------- N

Amount of HCl present = Strength of HCl × Equivalent

in the given solution weight.

= -----------N×36.5
= ----------- g/l

RESULT
Strength of the given HCl solution = ---------- N
Amount of HCl present in the given solution = --------g/l

15
 DETERMINATION OF TOTAL, TEMPORARY & PERMANENT HARDNESS
BY EDTA METHOD

Exp. No. 5 Date:

AIM
To estimate the amount of total, temporary and permanent hardness in the given sample
of hard water. A standard hard water of………N is provided.

PRINCIPLE
The estimation is based on complexometric titration. The total hardness of water is
estimated by titrating it against EDTA using EBT indicator.
pH = 9-10
EBT+M n+
[EBT-M]
Unstable complex (Wine red colour)
pH = 9-10
[EBT-M] + EDTA [EDTA-M] + EBT
Stable complex Steel blue colour
EBT indicator forms wine red coloured complex with hardness causing metal ions present in
water. On addition of EDTA, metal ions preferably form complexes with EDTA and steel blue
EBT indicator is set free. Therefore change of colour from wine red to steel blue denotes the
end point.
Temporary hardness is removed by boiling the water.
Ca (HCO3)2 CaCO3 ↓+CO2 +H2O
Mg (HCO3)2 Mg (OH)2 ↓ +2CO2 
The precipitate is filtered and the remaining permanent hardness is estimated using EDTA.

PROCEDURE
TITRATION I
STANDARDISATION OF EDTA
Pipette out 20ml of standard hard water into a 250ml conical flask. Add 5ml of
ammonia buffer solution and 4-5 drops of Eriochrome Black-T indicator. Fill the burette with
EDTA solution. Titrate the conical flask solution against the EDTA. The change in colour from
wine red to steel blue is the end point. Repeat the titration to get concordant values. Let the
titre value be V1ml.

TITRATION II
DETERMINATION OF TOTAL HARDNESS
Pipette out 20ml of the sample hard water into a clean conical flask. Add 5ml of
ammonia buffer solution and 4 -5 drops of Eriochrome Black-T indicator. Titrate the
wine red colour solution against the EDTA taken in the burette. The appearance of steel
blue colour is the end point. Repeat the titration to get concordant values. Let the titre
value be V2ml.
16
TITRATION III

DETERMINATION OF PERMANENT HARDNESS

Take 100ml of hard water sample in a 250ml beaker and boil gently for about
20 minutes. Cool, filter it into a 100ml standard flask and make the volume up to the
mark. Pipette out 20ml of boiled hard water into a clean conical flask. Add 5ml of
ammonia buffer solution and 4 -5 drops of Eriochrome Black-T indicator. Titrate the
wine red coloured solution against the EDTA taken in the burette. The appearance of
steel blue colour is the end point. Repeat the titration to get concordant values. Let the
titre value be V3 ml.
The temporary hardness is calculated by subtracting permanent hardness from total
hardness.

RESULT

(i) Amount of total hardness present in the given sample water = -----ppm (or)
mg/ l
(ii) Amount of permanent hardness present in the given sample water = ----ppm (or)
mg/ l
(iii) Amount of temporary hardness present in the given sample water = ----ppm (or)
mg/ l

17
SHORT PROCEDURE
TITRATION I TITRATION II TITRATION III
Determination of
CONTENTS Standardisation of Determination of total
permanent hardness
EDTA hardness
(Std. EDTA Vs Boiled
(EDTA Vs Std. hard (Std. EDTA Vs sample
hard water )
water) hard water )
Burette solution EDTA solution Std. EDTA solution Std. EDTA solution

Pipette solution 20ml Standard hard 20ml Sample hard water 20ml Boiled hard water
Water
Additional 5ml ammonia buffer 5ml ammonia buffer 5ml ammonia buffer
solution

Indicator 4-5 drops EBT 4-5 drops EBT 4-5 drops EBT

End point Wine red to steel blue Wine red to steel blue Wine red to steel blue
colour colour colour

TITRATION I
STANDARDISATION OF EDTA
Std. hard water Vs EDTA Indicator: EBT

S.No. Volume of Burette Reading (ml) Volume Concordant

Std. hard Initial Final of EDTA value (ml)
water (ml) (V1) ml

Calculation:
Standardisation of EDTA
Volume of Std. hard water (V1) = 20 ml
Strength of Std. hard water (N1) = ------ N
Volume of EDTA( V2 ) = ------ ml
Strength of EDTA ( N2) = ------ ? N
= ( 20 x N1 )/ V2

= ------ N
Strength of EDTA = ------ N

18
TITRATION II
DETERMINATION OF TOTAL HARDNESS
Std. EDTA Vs Sample hard Water Indicator: EBT
S.No. Volume of Burette Reading (ml) Volume of Concordant
sample hard Initial Final EDTA (V 2) ml value (ml)
water (ml)

Calculation:
Estimation of total hardness

Volume of EDTA( V1 ) = --------- ml

Strength of EDTA ( N1) = ----------N (From the titration I)
Volume of Sample hard water (V2) = 20 ml
Strength of Sample hard water (N2) = ---------?

N2 = (V1 × N1)/ 20

Strength of Sample hard water = --------- N.

Total hardness of the hard water sample = Strength of the hard water sample
×Eq.wt. of CaCO3

= --------- × 50 g/l

Therefore, Total hardness = --------- × 1000 ppm or mg/l

TITRATION III

DETERMINATION OF PERMANENT HARDNESS

Std. EDTA Vs Boiled hard water sample Indicator: EBT
S.No. Volume of Burette Reading (ml) Volume of Concordant
boiled hard Initial Final EDTA (V3) value (ml)
water (ml) ml

19
Calculation
Estimation of permanent hardness of the hard water
Volume of EDTA( V1 ) = ------ ml
Strength of EDTA ( N1) = ------ N (From the titration I)
Volume of boiled hard water sample (V2) = ------ 20 ml
Strength of boiled hard water sample (N2) = ?
N2 = (V1× N1 )/ 20
= N
Strength of boiled hard water sample = ------ N.

Permanent hardness = Strength of the boiled hard water sample × Eq.wt of CaCO3
= ------ × 50 g/l

Therefore, Permanent hardness of the hard water sample =….. × 1000 ppm or mg/l

Calculation of temporary hardness

Temporary hardness of the given sample of water = Total hardness – Permanent hardness

= ------------ ppm

20
 DETERMINATION OF DISSOLVED OXYGEN IN WATER SAMPLE
(WINKLER’S METHOD)

Exp. No. 6 Date:

AIM
To determine the amount of dissolved oxygen (DO) in the given water sample
by Winkler’s method. A standard solution of potassium dichromate of strength -------N is
provided.

PRINCIPLE
There are two methods, widely used to determine DO. They are,
(a) Winkler’s method by iodometry
(b) Electrometric method using a membrane electrode

Winkler’s method
DO in water reacts with Mn2+ ions in alkaline medium to form a brown colour basic
manganic oxide.
MnSO4 + 2 KOH Mn(OH)2 + K2SO4
2Mn (OH)2 + O2
-
2 MnO(OH)2 ↓(brown precipitate)
Manganic oxyhydroxide
This brown precipitate dissolves in con. H2SO4 and liberates iodine with KI. The Iodine
liberated is equivalent to the initial amount of DO present in the given water sample.
MnO(OH)2 + H2SO4 MnSO4 + 2H2O + [ O ] (Nascent oxygen)
2 KI + H2SO4 + [ O ] K2SO4 + H2O + I2 (Liberated Iodine)
The liberated iodine is estimated by titration with sodium thiosulphate.
I2 + Na2S2O3 Na2S4O6 + 2 NaI
[Note: Starch + I2 Blue coloured complex]

The stoichiometric expression relating DO and sodium thiosulphate is

1 ml of 0.0125N Na2S2O3  0.1 mg DO
Sodium thiosulphate (being a secondary standard) is standardised iodometrically using
standard K2Cr2O7.
Iodometry:(oxidant + excess I- )  I2 (liberated) Vs S2O32-
The net reaction is
Cr2O72- + 14H+ + 6I- 2Cr3+ + 7H2O + 3I2

In iodometric titrations, a slight excess of KI is added to ensure the completion of the

oxidation. Starch is added as an indicator which forms an intense blue coloured weak
adsorption complex with iodine liberated in low concentrations. The complex gets
readily broken when thio sulphate is added and hence a sharp colour change that is
disappearance of blue colour occurs at the end-point.

21
SHORT PROCEDURE
TITRATION I
TITRATION II
CONTENTS Standardisation of Na2S2O3
Estimation of D.O
Std. Na2S2O3 Vs Water
Std. K2Cr2O7 Vs Na2S2O3
Sample
Burette solution Na2S2O3 Std. Na2S2O3
20ml of treated water
Pipette solution 20 ml Std. K2Cr2O7
sample*
1 Test tube of 2N H2SO4 + 10ml
Additional solution -------
of 10% KI
Indicator Starch Starch
Disappearance of blue
End point Disappearance of blue colour
Colour
*200ml of sample water + 2ml of MnSO4 + 2ml of alkaline KI- Shaken for 5 min. A
brown gelatinous precipitate will be formed. Dissolve it with minimum amount of con.
Sulphuric acid to get a clear yellowish solution.

TITRATION I
STANDARDISATION OF SODIUM THIO SULPHATE
Std. K2Cr2O7 Vs Na2S2O3 Indicator: Starch
Volume of Burette Reading (ml) Volume of Concordant
S.No. std. K2Cr2O7 Na2S2O3
Initial Final value (ml)
(ml) (ml)

Volume of potassium dichromate (V1) = 20 ml

Strength of potassium dichromate (N1) = ------- N
Volume of sodium thio sulphate (V2) = ------- ml
Strength of sodium thio sulphate (N2) = -------?

N2 = V1N1/V2

N2 = 20 ml × ------- /-------

Strength of sodium thio sulphate (N2) = -------N

22
TITRATION II

ESTIMATION OF DO

Std. Na2S2O3 Vs Treated water sample Indicator :Starch

Volume of Burette Reading (ml) Volume of
Concordant
S.No. water sample std. thio
Initial Final value (ml)
(ml) (V2) ml

Volume of sodium thio sulphate (V1) = ---------ml

Strength of sodium thio sulphate (N1) = ---------(from the titration I)
Volume of DO water sample (V2) = 20 ml
Strength of DO water sample (N2) = ---------?
According to the law of volumetric analysis
V1N1 = V2N2

N2 = V1N1/V2

= --------- N

Amount of DO = Strength of DO in water sample × 8 g/l

= ---------- g/l
Amount of DO = ---------- × 1000 ppm (or) mg/l
= --------- ppm (or) mg/l
RESULT

The amount of DO present in the given water sample = --------- mg/l (or) ppm.

23
 ESTIMATAION OF ALKALINITY BY INDICATOR METHOD

Exp. No. 7 Date:

AIM
To determine the types and amounts of alkalinity in the given water sample. A
standard solution of NaOH of strength ------N is given.
PRINCIPLE
Alkalinity in water is due to the presence of soluble hydroxides, bicarbonates and
carbonates. Alkalinity can be determined by
(i) Potentiometric titrations
(ii) pH metry
(iii) Titrimetry using different indicators
Determination of various types and amounts of alkalinity is easily carried out by
titration with standard HCl employing the indicators phenolphthalein and methyl orange
independently or in succession.
The following reactions occur when different types of alkalinity are neutralized with
acid.
OH- + H+ H2O completed at pH 8.2-9.0 -------- (1)

CO32- + H+ HCO3- -------- (2)

HCO3- + H+ (H2CO3) H2O + CO2 completed at pH 4.2-5.5 -----(3)

Neutralization (1) & (2) will be notified by phenolphthalein end-point while all
the three will be accounted by methyl orange end-point. Bicarbonate in eqn.-3 may be due
to the existence of soluble free bicarbonate salts or bicarbonate resulting from half
neutralization of soluble carbonates (eqn.-2)
Various steps to be followed:
a) A known volume of water sample is titrated against std. HCl using phenolphthalein
indicator till the phenolphthalein end-point (P) and the titration is continued without
break using methyl orange indicator till the methyl orange end-point (M).
b) From the magnitudes of the P & M, the nature of alkalinity can be arrived as
follows:
c) (i) P = M => Presence of only OH-
(ii) 2P = M => Presence of only CO32-
(iii) P =0, M≠0 => Presence of only HCO3-
(iv) 2P > M => Presence of OH- & CO32-
(v) 2P < M => Presence of HCO3- & CO32-

(Mixture of OH- & HCO3- is not listed since they do not exist together and are
considered equivalent to CO32-).

24
 Relationshi Nature of Amount of individual OH- HCO3- CO32-
p between alkalinity alkalinities
P&M
P = M only OH- (P or M) × N ×50 xxx 0.0 0.0
20

2P = M only CO32- (2P or M) ×N × 50 0.0 0.0 xxx

20

P =0, M≠0 only HCO3- M × N × 50 0.0 xxx 0.0

20

2P > M OH- &CO32- OH- = (2P - M) × N ×50

20
xxx 0.0 xxx
CO 3
2-
= 2 (M-P) ×N × 50
20

2P < M HCO3&CO32- HCO3- = (M-2P) × N × 50

20
CO32- = (2P) × N × 50 0.0 xxx xxx
20

SHORT PROCEDURE:
TITRATION I TITRATION II
Standardisation of HCl Estimation of alkalinity in water
CONTENTS (Std NaOH Vs HCl) sample
(Std HCl Vs water sample)
Burette solution HCl Std. HCl

Pipette solution Std. NaOH Water sample

Indicator Phenolphthalein (i) Phenolphthalein

(ii) Methyl orange

End point Disappearance of pink colour (i) Disappearance of pink colour

(ii) Appearance of reddish orange
colour

Strength of HCl = --------- N

25
PROCEDURE:
TITRATION – I
STANDARDISATION OF HCl
Pipette out 20 ml of the given standard NaOH solution into a clean conical flask and add
2 drops of phenolphthalein indicator. Titrate the solution against the given HCl taken in
the burette. End point is disappearance of pink colour. Note the titre value from the
burette and repeat the titration to get concordant value.
TITRATION – II
ESTIMATION OF ALKALINITY IN WATER SAMPLE
Pipette out 20 ml of water sample into a clean conical flask. Add few drops of
phenolphthalein indicator and titrate the solution against the standardized HCl taken in
the burette. The end point is the disappearance of pink colour. Note the end point as P.
Then add few drops of methyl orange indicator in to the same solution. The solution
colour change to yellow. Continue the titration with same HCl solution without break
(without refilling the burette) till the end point is reached. The end point is change of
colour from yellow to reddish orange. Note the titre value and repeat the experiment to
get concordant value.

TITRATION I
STANDARDISATION OF HCl
Std. NaOH Vs HCl Indicator: Phenolphthalein
S.No. Volume of NaOH Burette Reading(ml) Volume of Concordant
(ml) Initial Final HCl value
(ml) (ml)
1
2
3

Volume of sodium hydroxide (V1) = 20 ml

Strength of sodium hydroxide (N1) =-------N
Volume of HCl (V2) =-------ml
Strength of HCl (N2) = ------?

N2 = V1N1/V2

= V1 × N1 / 20

Strength of HCl (N2) = -------N

26
TITRATION – II ESTIMATION OF ALKALINITY IN WATER SAMPLE
Std.HCl Vs Water sample Indicators: 1. Phenolphthalein
2. Methyl orange
S.No. Volume of Burette Reading Volume of Concordant
water Initial Final HCl (ml) Value (ml)
sample (ml)
P M P M P M

1
2
3
Phenolphthalein end point (P) =----------ml
Methyl orange end point (M) =----------ml
(i) Amount of OH- in water sample:
Volume of HCl (V1) = (2P-M) ml
Strength of HCl (N1) =-------N
Volume of water sample (V2) = 20ml
Strength of OH- in water sample (N2) = -------?
N2 = (2P-M) × -------N/20
Amount of OH-in water sample = N2 × 50 g/lit (50 is the eq.wt of CaCO3)
= N2 × 50 ×1000 mg/l.
= -------------- ppm.
(ii) Amount of CO32- in water sample:

Volume of HCl (V1) = 2(M-P) ml

Strength of HCl (N1) = -------N
Volume of water sample (V2) = 20 ml
Strength of CO32- in water sample (N2) = -------?
N2 = 2(M-P)×-------N/20
Amount of CO32- in water sample = N2 × 50 g/l.
= N2 × 50 ×1000 mg/l.

=-----------ppm.
RESULT

The types of alkalinity present in the water sample = ------ions.

The individual amount of alkalinity present in the water sample = -------ppm (or)mg/l

27
 ESTIMATION OF CHLORIDE CONTENT IN WATER SAMPLE BY
ARGENTOMETRIC METHOD [MOHR’S METHOD]

Exp. No. 8 Date:

AIM
To estimate the amount of chloride present in the given water sample, being
supplied with a standard solution of sodium chloride of strength ------- N .
PRINCIPLE
Generally water contains chloride ions in the form of NaCl, KCl,CaCl2, and
MgCl2. The concentration of chloride ions more than 250 ppm is not desirable for
drinking purpose. The total chloride ions can be determined by argentometric method
(Mohr’s Method).
In this method Cl –solution is directly titrated against AgNO3 using potassium
chromate (K2CrO4) as indicator

AgNO3 + Cl – AgCl ↓ + NO3–

(In water) (White ppt )
At the end point when all the Cl ions are removed. The yellow colour of
–

chromate changes to reddish brown due to the following reaction.

2AgNO3 + K2CrO4 Ag2CrO4 +2KNO3
(Yellow) (Reddish brown)
PROCEDURE
TITRATION I
STANDARDIZATION OF AgNO3
Wash the burette with distilled water and rinse with small amount of AgNO3
solution. Fill the burette with same solution up to the zero mark without any air bubbles.
Wash the pipette with distilled water and rinse with a small amount of standard NaCl
solution. Pipette out 20 ml of the solution in to a clean conical flask. Add 1ml of 2%
K2CrO4 indicator solution and titrate against AgNO3 taken in the burette. The end point is
the change of colour from yellow to reddish brown. Repeat the titration to get concordant
value.

TITRATION II
ESTIMATION OF CHLORIDE ION
Pipette out 20 ml of the given water sample in to a clean conical flask and add 1
ml of 2% K2CrO4 indicator solution. Then titrate the solution against standardized AgNO3
solution taken in the burette. The end point is the change of colour from yellow to reddish
brown. Repeat the titration to get concordant value.

28
SHORT PROCEDURE:

TITRATION I TITRATION II
Standardization of Estimation of
CONTENTS Silver Nitrate chloride
Std. NaCl Vs AgNO3 Std. AgNO3 Vs
Water Sample
Burette
AgNO3 Std. AgNO3
solution

Pipette solution 20 ml Std. NaCl 20 ml Water sample

Indicator 1 ml of 2% K2CrO4 1 ml of 2% K2CrO4

Appearance of
Appearance of reddish
End point reddish
brown colour
brown colour
TITRATION I
STANDARDISATION OF AgNO3:
Std. NaCl Vs AgNO3 Indicator: Potassium chromate
S.No. Volume of Burette Reading (ml) Volume of Concordant
NaCl (ml) Initial Final AgNO3 (ml) Value (ml)

Volume of sodium chloride (V1) = 20 ml

Strength of sodium chloride (N1) = -------N
Volume of silver nitrate (V2) =-------ml
Strength of silver nitrate (N2) =--------?

N2 = V1N1/V2
N2 = 20 ml × ………… /………
Strength of silver nitrate (N2) =........... N

29
TITRATION II
ESTIMATION OF CHLORIDE IN WATER SAMPLE
Std. AgNO3 Vs Water Sample Indicator: Potassium Chromate
Burette Reading (ml) Volume of
Volume of water Concordant
S.No. AgNO3
sample (ml) Initial Final Value (ml)
(ml)

Volume of silver nitrate (V1) = --------ml

Strength of silver nitrate (N1) = -------- N
Volume water sample (V2) = 20 ml
Strength of Chloride ions (in water) (N2) = ------N

N2 = V1 × N1
V2
Strength of Chloride ions (in water) (N2) = -------N

Calculation of amount of Chloride ions

Amount of chloride ions present in 1 litre of water sample

= Equivalent weight of Chloride ion (35.45) × Strength of chloride ions in water

= 35.45 × -------------------g

= -------------g

Amount of Chloride ions present in 1 litre of the water sample

= --------------g × 1000ppm

= -------------mg / l or ppm

RESULT

Amount of chloride ions present in the given water sample = ---------ppm

30
 DETERMINATION OF SODIUM AND POTASSIUM IN WATER SAMPLE BY
FLAME PHOTOMETRY
Exp. No. 9 Date:

AIM
To determine the amount of sodium and potassium present in the given water sample
using flame photometer.

PRINCIPLE
Flame photometry (or) Flame Emission Spectroscopy is based on the principle of
emission of certain radiation in the visible region by a metal atom. In this technique metal
atom is thermally excited from the ground state. The excited atom emits light of
particular intensity while returning to the ground state depending upon the concentration
of the metal ions. A water sample to be analysed is sprayed into the flame, where the
water evaporates leaving the fine salt particles. This salt decomposes into constituent
atoms, when they are heated to about 1700°C. The vapours containing metal atoms are
excited by the thermal energy of the flame to higher energy state.
When the electrons fall down from the excited state to ground state, they emit
radiation. The emitted radiation is measured and recorded. The emission spectrum for
each metal is different and its intensity depends on the concentration of the atoms in the
flame. Sodium produces a characteristic yellow emission at 589 nm. Potassium produces
a characteristic red emission at 766 nm.
Different standard solutions (say 1. 2, 4, 6, 8 & 10 ppm ) are prepared and the
calibration curve is drawn between concentration (ppm) Vs intensity of emitted light
(photometric readings).

PROCEDURE
Step 1: Preparation of stock Na+ solution
A stock solution of Na+ is prepared by dissolving 2.54 grams of NaCl in 1 litre of
distilled water
1 ml of stock solution = 1 ppm of Na+
From the stock solution, various concentrations are prepared (1, 2, 4, 6 & 8 ppm).
Step 2: Preparation of stock K+ solution
A stock solution of K+ is prepared by dissolving 1.809 grams of KCl in 1 litre of
distilled water
1 ml of stock solution = 1 ppm of K+

31
 From the stock solution various concentrations are prepared (1, 2, 4, 6, & 8 ppm)

Step 3: Working with instrument

The instrument is switched on. Air supply and gas supply are regulated. First
distilled Water is sent and ignition is started. After the instrument is warmed up for 10
min, the instrument is adjusted for zero reading in the display.
(a) Determination of sodium in the water sample
NaCl solution of 8 ppm is sent and the reading is adjusted for 100. Now the
instrument is said to be calibrated. The solution of NaCl of other known concentrations
(1, 2, 4 and 6 ppm) is sent one by one and the reading (intensity of emitted light) is noted.
The calibration graph is drawn between the concentrations Vs. intensity of the emitted
light (readings). Now the unknown water sample is sent and the intensity of emitted light
(reading) is noted. Then the concentration of sodium in the water sample is determined
from the calibration curve

(b) Determination of potassium in the water sample.

KCl solution of 8 ppm is sent and the reading is adjusted for 100. Now the
instrument said to be calibrated. The solution of KCI of other known concentration (1. 2.
4 and 6 ppm) is sent one by one and the reading is noted as before. The calibration graph
is drawn between the concentrations Vs. readings. Now unknown water sample is sent
and the reading is noted. Then the concentration of potassium in the water sample is
determined from the calibration curve.

32
Table -1: Preparation of various concentrations of Na+ and K+ solutions
S.No Volume of stock Volume of distilled Total volume Concentration
solution(ml) water (ml) (ml) in ppm
1
2
3
4
5

Graph: Calibration curve (Intensity Vs. Concentration)

Table- 2: Determination of Na+ in sample water

λ= 589 nm
Distilled water = Zero Readings
S.No Concentration of NaCl Intensity of emitted light(readings)
1 1 ppm
2 2 ppm
3 4 ppm
4 6 ppm
5 8 ppm
6 Unknown water sample

33
Table- 3: Determination of K+ in sample water
λ= 766 nm
Distilled water = Zero Readings
S.No Concentration of KCl Intensity of emitted light (readings)
1 1 ppm
2 2 ppm
3 4 ppm
4 6 ppm
5 8 ppm
6 Unknown water sample

RESULT
(a) The amount of sodium present in the water sample = ----------ppm
(b)The amount of potassium present in the water sample = -------ppm

34
DETERMINATION OF FLASH AND FIRE POINT OF LUBRICATING OIL
Exp. No. 10 Date:

AIM
To determine the flash point and fire point of the given lubricating oil or liquid fuels.

REAGENTS REQUIRED
Test oil/sample, solvent to clean and dry the cup.

PRINCIPLE
Flash point is the lowest temperature at which the fuel gives enough vapours that
ignite for a moment, when a small flame is brought near it.
Fire point is the lowest temperature at which the vapours of the oil burn
continuously for atleast 5 seconds, when a small flame is brought near to it. Generally,
the fire point is 5 - 40°C higher than the flash point. Though these points are not related
to the lubricating properties of oil, a Knowledge of these is helpful to provide safety
measures against the fire hazards during use and storage.

EXPERIMENTAL PROCEDURE
Flash and fire points are determined using Pensky-Marten’s apparatus.
1. The fuel sample is filled up to the mark in the oil cup and then heated by
heating the water bath by a burner.
2. Stirrer is worked between tests at a rate of about 1 to 2 revolutions per second.
3. Heat is applied so as to raise the oil temperature by about 5 C per minute
4. At every 1 C rise of temperature, flame is introduced for a moment by
working the shuttle.
5. The temperature at which a distinct flash appears is noted and it is the flash
point.
6. The heating is continued thereafter and the test flame is applied as before.
7. When the oil ignites and continues to burn for atleast 5 seconds, the
temperature reading is noted and is the fire point.

35
TABLE 1
S.No Temperature (0C) Inference (No cloud or pour observed)
1.
2.
3.
4.
5.
6.

RESULT
1. The flash point of the given lubricating oil = ...................°C
2. The fire point of the given lubricating oil = ...................°C

36
DETERMINATION OF CLOUD AND POUR POINT OF LUBRICATING OIL
Exp. No. 11 Date:

AIM: To determine the cloud point and pour point of the given lubricating oil/liquid fuel

PRINCIPLE
When a petroleum or a lubricating oil is cooled slowly under specified condition,
the temperature at which the paraffin wax or any other solidifiable material begins to
separate from the solution in the form of minute crystals, causing the oil to become less
transparent, cloudy or hazy in appearance and is known as cloud point of the oil.
The lowest temperature at which the oil ceases or stops to flow or pour is called
its pour point. Cloud and pour points indicates the suitability of lubricants in cold
conditions. Lubricant used in a machine working at low temperatures should possess low
pour point, otherwise solidification of lubricant will cause jamming of the machinery. It
has been found out that the presence of wax in the lubricating oil raises the pour point.

PROCEDURE
Determination of pour point is carried out with the help of pour point apparatus. It
consists essentially of a flat bottomed tube enclosed in an air jacket. The jacket is
surrounded by freezing mixture (ice+CaCl2) contained in a jar.
The tube is half filled with the oil and a thermometer is introduced in the oil. As
the cooling proceeds slowly, the temperature falls continuously and with every degree
fall of temperature of the oil, the tube is withdrawn from the air jacket for a moment
(about 2-3 seconds) and examined. It is then replaced immediately. The temperature at
which cloudiness appeared is recorded as the cloud point. After this, the cooling is
continued and the test tube is withdrawn after every 3°C fall of temperature and tilted to
observe the flow or pour of the oil. The temperature at which does not flow in the test
tube, (even when horizontal for a few seconds) is recorded as the pour point.

RESULT
1. The cloud point of the given lubricating oil = --------------°C.
2. The pour point of the given lubricating oil = --------------°C.

37
 DETERMINATION OF CORROSION RATE ON MILD STEEL BY WEIGHT
LOSS METHOD
Exp. No. 12 Date:

AIM
Determine the rate of corrosion of mild steel specimen in hydrochloric acid of different
concentrations at room temperature by weight loss med

MATERIALS REQUIRED
1. Mild steel pieces
2. Electronic balance
3. Abrasive (sand) paper
4. Air drier
5. Stop watch
6. Hydrochloric acid

PRINCIPLE
Almost all metals undergo corrosion. Corrosions is an undesirable and slow
process. The cost of replacement of materials and equipments lost through corrosion is
estimated to be more than one lakh crore rupees per year. Thus, corrosion is regarded as a
cancer that destroys economy and equipments.
Generally metal surfaces are covered with impurities like rust and scales. These
impurities at the time of coating, will produce porous and discontinuous coating. In order
to obtain an adherent cohesive, smooth and uniform coating, the impurities must be
completely removed by dipping them in an acid. This is known acid cleaning or pickling.
Pickling is generally employed to remove the scale by oxidation of metal.

Dilute hydrochloric acid is used as pickling solution. By dipping the metal plate in
the acid, the metal ions along with rust get dissolved. Such dissolution is called
corrosion. It is observed that as the time of dipping in acid increases and the acid
concentration increases, the rate of corrosion also increases.

PROCEDURE
Mild steel specimens of known dimensions are taken and are washed thoroughly
with distilled water and are air dried. The initial weight of the specimens is noted (w1 g).
Different concentrations (1 N, 2 N, 3 N, 4 N, 5 N) of hydrochloric acid solutions
are prepared. They are known as pickling solutions.
The mild steel specimens are dipped in 100 mL of various hydrochloric acid
solutions for about 30 minutes. After that they are taken out and are washed with distilled
water thoroughly and are air dried. Again the specimens are weighed. The final weights
38
are noted (w2 g). From the weight loss (w1- w2), the rate of corrosion can be calculated
using the formula.

Where,
w1 = Initial weight of the specimen
w2 = Final weight of the specimen
D = Density of the specimen
For mild steel, D 7.85 g/cm3
T = Time of exposure in (hour)
A = Area of the specimen in (inch)2

As the corrosion is a slow process, the other units used for rate of corrosion are

(a) millimeter per year (mpy)

(b) inch per year (ipy)
(c) mg per dm per day (mdd)

Table-1: Corrosion rate – Weight loss method

S.No Initial Final Weight Concentration Time of Area

Weight Weight loss of HCl (N) Exposure (inch)2
w1 g w2 g (w1 - w2) g (hour)

= ---------inch/year
RESULT
Rate of corrosion= ------------inch/year

39
 DETERMINATION OF MOLECULAR WEIGHT OF POLYMER BY
VISCOMETRY METHOD

Exp. No. 13 Date:

AIM
To determine the molecular weight (M) and degree of polymerization (DP) of a
polymer by viscosity average method.

PRINCIPLE
Viscosity average method is based on the flow behavior of polymer solutions.
According to Mark – Hawnik equation, the intrinsic viscosity of a polymer is given as
[]int = KMa

Where,
M = molecular weight of the polymer
K & a are constants for a particular polymer – solvent system
[]int = Intrinsic viscosity = [sp/C]C=0 = [r/C]C=0
sp = specific viscosity = r – 1
r = relative viscosity = /0 = t / t0

Since accurate measurement of absolute viscosity is a difficult task, relative viscosity is

taken into account for finding the molecular weight.
 = Viscosity of the polymer solution
0 = Viscosity of the pure solvent
t = flow time of the polymer solution
t0 = flow time of the pure solvent

The flow time of the polymer solution (t) and that of the pure solvent (t0) are found
experimentally and substituted to get sp , r and []int.
Knowing K & a, molecular weight of the polymer solution is calculated.
DP = M / m (M= mol.wt of polymer, m = mol. wt of monomer).

40
Solvent used = Water

K of the polymer solvent system = ------

a of the polymer-solvent system = ------

Volume of liquid taken for finding the flow time = 10ml

Flow time of the solvent (t0) = ------ sec

Flow
Conc.
S.No. time r = t / t 0 sp=r -1 sp / C
g/dl or (%)
(t)sec

S.No. Polymer Solvent K x 10-5 a

1 Polyvinyl alcohol Water 45.3 0.64

2 Polyvinyl pyrrolidone Water 39.3 0.59

3 Polystyrene (atactic) Benzene 11.5 0.73

4 Polystyrene (isotactic) Benzene 10.6 0.735

41
PROCEDURE
Accurately take 1g weight of polyvinyl alcohol, dissolve it in water and make up
to 100ml (1dl) in a standard flask. From the solution, Prepare the polymer solutions of
concentration 0.1g/dl,0.2g/dl,0.3g/dl,0.4g/dl and 0.5g/dl using the relation V1N1 = V2N2

[E.g. for preparing 100ml of 0.2g/dl from 1g/dl solution x ml polymer is made up to
100ml with water where x is caculated using the relation, x ml × 1 g / dl = 0.2
g / dl × 100ml]
Rinse the Ostwald viscometer with water, and then fill with 10ml of distilled water.
Using a rubber bulb, suck the water in the viscometer to the upper bulb. Allow the water
to flow from the upper mark till the lower mark in the viscometer. Using a stop clock
measure the time taken for water to flow from the upper mark to the lower mark and note
the value as t0 sec.

Drain the water from the viscometer completely and take 10ml of the polymer solution of
0.1g/dl concentration in it. Note the flow time of the polymer solution as t sec. Repeat the
procedure with the other solutions of the polymer.

Calculate sp / c from the values of t and t0, and draw the graph taking sp / c Vs c.
Extrapolate the straight line obtained to zero concentration. The intercept value is equal
to []int. Calculate the molecular weight of the polymer (M) using the formula

[]int = KMa (constant K and a are given in the table)

Calculate the degree of polymerization from the values of M and m ,

RESULT

The molecular weight of the given polymer =

The degree of polymerization of the polymer =

42
 [] = KM a

Ma = []/K

a log M = log[] - log K

M = antilog { }
a

Degree of polymerization = Molecular wt of the polymer

Mol.wt of the repeating units

DP = MV
Mol.wt of the repeating units

ADSORPTION OF ACETIC ACID BY CHARCOAL

43
Exp. No. 14 Date:

AIM
To study the adsorption of acetic acid aqueous solution by activated charcoal and
examine the validity of Fruendlich’s adsorption isotherm.

PRINCIPLE
The phenomenon of higher concentration of a species at the surface of other
material 9than in its bulk) is termed as adsorption. Adsorption is a surface phenomenon,
finding applications in the fields of catalysis, water softening, chromatography etc. the
species held together is called adsorbate and the material having the capacity to hold
other species on its surface is called adsorbent. Adsorbate may be in liquid/gas phase and
adsorbent in solid/liquid phase. Greater the area of the adsorbate, greater is its adsorptive
capacity. The variation of extent of adsorption (mass of adsorbate per unit mass of
adsorbate, x/m) with the concentration (pressure, if in gaseous phase) of the adsorbate (C)
at constant temperature is called adsorption isotherm. In the adsorption of acetic acid on
charcoal, Freundlich adsorption isotherm, i.e. x/m = KC1/n (K and n are constants
characteristic of the combination) can be applied. Freundlich isotherm holds good only at
low temperatures the plot x/m Vs log c is linear from which k and n can be calculated.

PROCEDURE
Take 50, 40, 30, 20 and 10 ml of 0.1 n acetic acid solutions (to be standardized) in
5 stopper bottles (numbered 1 to 5) and add 0, 10, 20, 30 and 40 of distilled water
respectively in these bottles. Add 0.5 gm of activated charcoal in each bottle and shake
vigorously the bottles for an hour. Filter the solution from each bottle and titrate a known
volume of each filtrate (say 10 ml) against NaOH solution using phenolphthalein
indicator. The end point is the appearance of pink colour. Calculate the amount of acetic
acid adsorbed per gram of adsorbent (charcoal) and the equilibrium concentration of the
acid. Draw the graphs of x/m Vs C and log x/m Vs log C. the plot of log x/m against log
C is a straight line, whose slope and Y-intercept give the values of Freundlich constants
‘n’ and ‘k’.
RESULT
The Freundlich isotherm is verified for the adsorption of acetic acid on charcoal
and the constants n and k were found to be ………………… and ………………….
respectively.

44
 Table: 1
Bot Mass of Conc. Of Conc. Of Acetic acid adsorbed Log C
tle charcoal AcOH before AcOH after x = (C1-C2) × 60 ×
No (gm) adsorption adsorption
(C1N) (C2N)

Table: 2
Bottle Volume Burette Reading Volume of Concordant Indicator
No of AcOH Initial Final NaOH value

Observation and Calculations:

Concentration of acetic acid before adsorption = 0.1 × , Where V  Volume of acetic
acid taken in the stopped bottle
Let, V1 ml of filtrate from the bottle no: --------------- consume V2 ml of 0.1 N NaOH
V1 N1 = V2 × 0.1
N1 = Normality of acetic acid after adsorption
Hence the amount of acetic acid adsorption by the charcoal is 0.1 – N1 g equivalents per
liter

Model Graph:

45
 DETERMINATION OF PHASE CHANGE TEMPERATURE OF A SOLID
Exp. No. 15 Date:

Aim - To determine the melting point of given solid substance.

Requirements – Given Solid Substance, Capillary Tube, Paraffin,

Laboratorythermometer.

Theory- The change from solid to liquid state of a compound in heating is called
melting and the temperature at which a solid in its pure form melts is called the melting
point. Every pure solid has a characteristics melting point therefore determination of
melting point helps in identification of the compound. Presence of impurities lowers the
melting point of the solid. Thus Melting point also serves as a criterion of purity of a
compound.

Procedure-

1. Take a fine capillary of length 5-6cm. seal its one end by inserting the end of the
capillary tube horizontally into the extreme edge of a small steady Bunsen flame for a
few seconds, rotating the capillary meanwhile.

2. Take a small quantity of the compound whose melting point is to be determined on a

porous plate and powder it with aspatula.

3. Introduce the powdered compound in the capillary tube by introducing the open end
of the capillary tube into the powdered compound and gently rotating it.
Gentlytapthecapillarytubeagainsttheporousplatesothatthecompoundsinks
into the closed end. Repeat the procedure of introducing and tapping three to four times.

4. Moisten the bulb of thermometer with Conc. Sulphuric acid or liquid paraffin and
46
 attach the capillary to the lower end of thethermometer.

5. Place the thermometer with the capillary tube in the melting point apparatus
containing at least two third of its volume liquid paraffin in such a way that theclosed
end of the capillary remains below the surface of Liquidparaffin.

6. Now heat the beaker gently and note down the temperature from time to time and
finally note down the temperature at which the compound starts melting and
completely melts.

7. Repeat the experiment with a new capillary tube and fresh quantity of the
substance.

Observations-

Melting point

1……………………0C

2……………………0C

3……………………0C

Mean Melting point = (t1+t2+t3)/3 0C

Precaution-

1. The capillary tube is filled one third of itslength.

2. The rate of heating should be controlled. It should be very slow near the melting
point so that the melting point can be recordedaccurately.

RESULT
The melting point of given solid substance =

VIVA-VOCE – QUESTION BANK

47
Experiment : 1
CONDUCTOMETRIC TITRATIONS
1. Define the term conductivity.
2. Give the unit of conductance.
3. What is specific conductance?
4. Define Equivalent conductance and molar conductance.
5. Explain why do we get “V” shaped graph for conductometric titration of HCl Vs
NaOH?
6. List out the advantages of conductometric titrations.
7. Draw the rough graph obtained by plotting conductance Vs Vol of NaOH in the
estimation of mixture of acids (SA+WA).
8. Which acid will be neutralised first when a mixture of HCl and acetic acid is
titrated against NaOH?
9. Why the conductance decrease until the first neutralization point?
10. The second neutralization point conductance increases slowly and then
shows steep rise. Explain
11. Explain the graph obtained by plotting Conductance against volume of Na2SO4 in
precipitation titration

Experiment:2
POTENTIOMETRY – REDOX TITRATION

1. What is an electrochemical cell?

2. What is single electrode Potential?
3. What is standard electrode potential?
4. Define reduction potential
5. Mention the factors affecting electrode potential?
6. Give the formula to calculate EMF of a cell
7. Name the electrodes acting as cathode and anode in the experiment
8. What is redox titration?
9. Explain the redox reaction that takes place when FeSO4 is titrated against K2Cr2O7.
10. Platinum electrode is a oxidation – reduction electrode in the presence of Fe2+ and
Fe3+ Why?
11. What is the reduction potential of calomel electrode?
12. Give the advantages of Potentiometric titrations.
13. What is calomel electrode?

Experiment: 3
ESTIMATION OF IRON BY SPECTROPHOTOMETERY

1. What is the principle of spectrophotometry?

2. How is the light from a monochromatic source gets distributed on falling upon
medium?
3. What is absorbance?
4. What is transmittance?
5. What is a spectrophotometer and spectrophotometry?
6. State Beer-Lamberts law?
7. What is the role of KCNS in the estimation of iron by spectrophotometry?
8. Why is the monochromator adjusted for  = 480nm during the estimation of iron?
48
9. Mention the working range of wave length of spectrophotometer?

Experiment: 4
pH METRY

1. Define pH
2. Give the principle of pH metry ?
3. Name the electrodes used in the determination of pH of a solution.
4. Which electrode act as anode and which acts as cathode? Why?
5. What is the effect of temperature on pH?
6. What is the effect of dilution on pH of an acid solution?
7. What is the pOH of pure water at 25°C
8. What is a combined electrode?
9. What is the significance of pH titration?
10. Brief the function of calomel electrode?
11. What are the pH of lime juice, blood and de-ionised water?

Experiment: 5
ESTIMATION OF HARDNESS IN WATER

1. What is Hardness?
2. What are the two types of hardness?
3. Write the structure of EDTA.
4. Give the reaction between EBT and hardeness causing ions.
5. What is the pH range for complex stability in EDTA method?
6. What is the buffer used in the titration?
7. Give reason for the formation of red and blue colours in the titration.
8. What are the disadvantages of hardness?
9. What may be the range of hardness in a portable water sample?
10. What is the need of filtration during the experiment?
11. What are the units by which hardness is expressed?
12. What is the other name for Eriochrome black T?
13. Why is CaCO3 used as reference in hardness calculations?

Experiment: 6
ESTIMATION OF DISSOLVED OXYGEN

1. What is the extent of oxygen dissolution in water at 30°C?

2. What is the need of determining the amount of DO in water?
3. What is Winkler’s reagent?
4. What are the reactions involved in DO estimation?
5. Why do we dissolve the precipitate formed in Conc.H2SO4?
6. What are the principle behind iodometry and iodimetry?
7. What is the name of the brown precipitate we get in the estimation?
8. How can we avoid dissolution of O2 in water?
9. Why should we put stopper on the bottle used for DO estimation?
10. Explain the process of Winkler’s method of estimation of DO

49
Experiment : 7
ESTIMATION OF ALKALINITY IN WATER

1. What is alkalinity?
2. What are the ions responsible for alkalinity in water?
3. What are the five possible alkalinities in water?
4. What are the indicators used in the titration?
5. What is the equivalent weight of CaCO3.
6. What is the reaction of Phenolphthalein end point?
7. What is ppm?
8. Explain Lewis concept.
9. Expalin Bronsted – Lowry concept.
10. What is the colour of phenolphthalein in acidic and basic medium?
11. What is the colour of methyl orange in acidic and basic medium?

Experiment: 8.
ESTIMATION OF CHLORIDE CONTENT IN WATER SAMPLE BY
ARGENTOMETRIC METHOD [MOHR’S METHOD]

1. Explain the principle behind the argentometry?

2. Why do we get a blurred solution during the titration?
3. What type of medium is preferred for chloride estimation?
4. What is the colour change that infers the end point?
5. What is the relationship between ppm and g/ml?
6. What are the different sources of chloride in water?
Experiment: 9.
DETERMINATION OF SODIUM AND POTASSIUM IN WATER SAMPLE BY
FLAME PHOTOMETRY

1.What is the principle of flame photometry?

2.What are the steps involved in FPM?
3.What is the use of thermal excitation process here?
4.What are the components of flame photometry?
5.What are the other names of grating?
6.How will you prepare a standard solution of a salt?
7.What are the applications of flame photometry?
8.What is the possible interference in FPM?
9.What are the limitations of FPM?
10.What are the colours of the flame for Na?
11.What is absorbance?
12.What is molar extinction coefficient?
13.State Beer-Lambert’s law.
14.Why is the colour measured at 480 nm?
15.What is transmittance?

Experiment: 10.
50
DETERMINATION OF FLASH AND FIRE POINT OF LUBRICATING OIL
1. What is flash point?
2. Define fire point.
3. Give some example of lubricating oil.

Experiment: 11.
DETERMINATION OF CLOUD AND POUR POINT OF LUBRICATING OIL
1. What is cloud point?
2. State pour point.
3. Write the uses of lubricating oil.
4. What are the types of lubricating oil.

Experiment: 12.
DETERMINATION OF CORROSION RATE ON MILD STEEL BY WEIGHT
LOSS METHOD
1. What is weight loss method?
2. Define corrosion.
3. What are the types of corrosion?
4. What is the formula for Rate of Corrosion?
5. What is Inch/Year?
6. Explain about acid pickling
7. What is Rust. Give its formula?
8. Which is regarded as a cancer that destroys economy and equipments.?
9. Define Pilling Bedworth Ratio.
10. What is galvanic corrosion?
11. What is Decarburization?
12. What is Hydrogen embrittlement.

Experiment: 13.
DETERMINATION OF MOLECULAR WEIGHT OF POLYMER BY
VISCOMETRY METHOD

1. What is polymer?
2. Write the principle of viscometry.
3. Mention the formula used in molecular weight calculation.

Experiment: 14.
ADSORPTION OF ACETIC ACID BY CHARCOAL
1. Define adsorption.
2. What is the role of acetic acid in this experiment?
3. Write the application of charcoal.
4. What are the uses of charcoal in various fields?

Experiment: 15.

51
DETERMINATION OF PHASE CHANGE TEMPERATURE OF A SOLID
1. Define melting point.
2. How does the determination of melting point help us to know about the purity of
compound?
3. What is the effect of impurity on melting point of solid
4. How is determination of melting point useful?
5. Why different solids have different melting point?
6. Can any other liquid be used in the place of paraffin to determine the melting
point?

52