St.

MARTIN’S ENGINEERING COLLEGE

Dhulapally-500014, Secunderabad

ENGINEERING CHEMISTRY

LAB MANUAL
A.Y:2018-2019
SUBJECT CODE:106BS

LIST OF EXPERIMENTS:

1
1. Determination of total hardness of water by complexometric method using EDTA

2. Determination of chloride content of water by Argentometry

3. Estimation of an HCl by Conductometric titrations

4. Estimation of Acetic acid by Conductometric titrations

5. Estimation of HCl by Potentiometric titrations

6. Estimation of Fe2+ by Potentiometry using KMnO4

7. Determination of rate constant of acid catalysed hydrolysis of methyl acetate

8. Synthesis of Aspirin and Paracetamol

9. Thin layer chromatography calculation of Rf values. eg ortho and para nitro phenols

10. Determination of acid value of coconut oil

11. Verification of freundlich adsorption isotherm-adsorption of acetic acid on charcoal

12. Determination of viscosity of castor oil and ground nut oil by using Ostwald’s viscometer.

13. Determination of partition coefficient of acetic acid between n-butanol and water.

14. Determination of surface tension of a give liquid using stalagmometer

2
1.DETERMINATION OF TOTAL HARDNESS OF WATER BY COMPLEXOMETRIC
METHOD USING EDTA

AIM:
To determine the total hardness of water by EDTA method.

REQUIRMENTS

Burette, Conical flask, PipetteStandard ZnSO4 solution, EDTA Solution, Ammonia– Ammonium chloride
buffer and water Sample

INDICATOR
Eriochrome black –T (EBT)

END POINT
The end point is noted when the colour of the solution changes from wine red to blue

PRINCIPLE
The hardness of water is due to the presence of salts of Ca2+ and Mg2+. The bicarbonates of Ca2+ and Mg2+ impart
temporary hardness to water which can be removed by boiling. The amount of Ca2+ and Mg2+ is estimated by
complexometric method using EDTA. The obtained value gives the total hardness. The permanent hardness is
determined first by precipitating the bicarbonates of Ca2+ and Mg2+ by heating and filtering off and the filtrate is
titrated with EDTA. The temporary hardness is obtained by subtracting permanent hardness from total hardness.

EDTA Titrations (or complexometric titrations):

The titrations involving EDTA as a complexing agent are known as “EDTA Titrations” (or) “Complex Formation
Titrations”. EDTA stands for
‘Ethylene Di-amine Tetra Acetic acid” or “Di-amino Ethane Tetra Acetic Acid.

The structure of EDTA is given by

EDTA forms complexes with metal ions like Ca2+, Mg2+, Ba2+, and Sr2+ in aqueous solution. Complexometric
titration is the titration of metal ion with a reagent, usually EDTA, which forms chelated complex with a metal. The
common indicator used is Eriochrome Black-T Indicator (EBT), at the end point the colour changes from red to blue.

3
 Na+ Na+

Disodium salt of
EDTA

Ethylene diamine tetra acetic acid [EDTA] forms colorless stable complex with Ca+2 and Mg+2 ions present in water
at pH 9-10. To maintain pH of the solution at 9-10, NH3-NH4Cl buffer solution is used. Eriochrome black –T (EBT)
is used as indicator. The hard water when treated with (EBT) in presence of buffer solution forms unstable wine red
color complex with Ca+2 and Mg+2 ions present in water.
The stability of a metal indicator complex is less than that of metal EDTA complex. Hence during the titration,
EDTA extracts the metal ions from the metal ion- EBT indicator complex and forms stable colorless metal EDTA
complex releasing free indicator. Hence the end point of the titration is the color change from wine red to blue color.

4
PROCEDURE:
PART A: STANDARDISATION OF EDTA SOLUTION
10ml of standard Zn2+ solution is pipette out into a well cleaned conical flask. To it one drop of indicator and 1
ml of buffer are added. The solution is diluted to 20ml using distilled water. Then the solution is titrated against
EDTA until wine red color changes from red to blue. This is taken as end point. Titrations are repeated until two
successively concurrent values are obtained. The molarity of EDTA is calculated by using the formula
V1M1=V2M2.
TABULATION :

PART A: STANDARDISATION OF EDTA SOLUTION

Volume of standard Burette readings (ml) Volume of EDTA

S.NO
Zn+2 solution (ml) Initial Final run down ‘x’ (ml)
1 10
2 10
3 10

M1V1=M2V2

M1 = Molarity of standard Zn2 + solution

V1 = Volume of standard Zn2 + solution
V2 = Volume of EDTA rundown
M2 = Molarity of EDTA Solution
M1 V1
M2 =
V2

PART B: DETERMINATION OF TOTAL HARDNESS OF TAP WATER

50ml of tap water is taken into a well cleaned conical flask. To it 2ml of buffer and 2-3 drops of EBT indicator
are added. The color of resulting solution is wine red. The contents of the conical flask are titrated against EDTA
which is taken in the burette until the colour of the solution changes from wine red to blue. This is the end point.
Repeat the titration until two successively concurrent values are obtained.
Burette readings (ml) Volume of EDTA run
S.NO Volume of tap water (ml)
Initial Final down ‘x’ (ml)
1 20 0
2 20 0
3 20 0
M2V2 = M3V3
M2 = Molarity of EDTA solution
V2 = Volume of EDTA rundown
M3 = Molarity of tap water
V3 = Volume of tap water
M2 V2
M3 = .
V3
Total hardness of tap water = M3×100×1000 mg/litre or ppm

5
PART C:DETERMINATION OF PERMANENT HARDNESS OF WATERPlace 100ml of water sample in a
250ml beaker and boil gently for 20-30 minutes. Cool and filter, collect the filtrate into a 250ml standard flask. Make
up the solution to the mark by adding distilled water and shake the solution well. Pipette out 50ml of this made up
solution into a clean conical flask, which has been rinsed with distilled water. Add 2ml of pH = 10 buffer solution
and 2 to 3 drops of EBT indicator.Titrate this solution against the standard EDTA solution until the colour changes
from wine red to blue. Note down the reading, repeat the process to get successively two concurrent titre values.
Calculate the permanent and then temporary hardness as parts per million of CaCO3.

Volume of boiled water Burette readings (ml) Volume of EDTA run down
S.NO Initial Final
(ml) ‘x’ (ml)
1 20 0
2 20 0
3 20 0

M2 = Molarity of EDTA

M4 = Molarity of boiled water

V2 = Volume of EDTA

V4 = Volume of boiled water = 20ml

M2V2 = M4V4

𝑀4
Molarity of boiled water M4= × 𝑉4
𝑉2

Permanent hardness of tap water = M4 × M.W of CaCO3 ×1000

= M4 × 100×1000 = ………..mg/litre or ppm

Temporary hardness = Total hardness – Permanent hardness

RESULT:

(i) Amount of total hardness of the given sample water = ---------- ppm
(ii) Amount of permanent hardness of the given sample water = --------- ppm
(iii) Amount of temporary hardness of the given sample water = -------- ppm

6
 1. DETERMINATION OF CHLORIDE CONTENT IN WATER BY ARGENTOMETRIC
METHOD (MOHR’S METHOD)

Aim

To determine the amount of chloride present in 100 ml of given water sample being supplied with
standard solution of sodium chloride of strength 0.1N and an approximately N/20 solution of silver nitrate.

Requirments

Burette,pipette,conical flask ,burette stand,std Nacl solution, AgNo3 solution, 2%K2CrO4 indicator

Principle

Generally water contains chloride ions (cl-) in the form of NaCl, KCl,CaCl2 and MgCl2.The
concentration of chloride ions in water ,more than 250ppm,is not desirable for drinking purpose.The total
chloride ions can be determined by argentometric method ( Mohr’s Method).

In this method Cl- ions are removed. The yellow colour of chromate changes into reddish brown due
to the following reaction.

2AgNo3 + K2Cro4-----------> AgCl +2KNo3

At the end point, when all the cl- ions are removed.The yellow colour of chromate changes into reddish
brown due to the following reaction.

2AgNo3 +K2Cro4 ----------> Ag2Cro4 + 2KNO3

(Reddish brown precipitate)

Procedure

Titration –I Standardisation of Silver Nitrate

The burette is washed well with distilled water and rinshed with the small amount of AgNo3
solution.It is then filled with the same solution upto the zero mark without any air bubbles.

The pipette is washed with distilled water and rinshed with the small amount of Standard Nacl
solution.20ml of this solution is pipette out into a clean conical flask. 1ml of 2% K2CrO4 indicator solution
is added and titrated against AgNo3 solution taken in the burette. The end point is the change of colour
from Yellow to reddish brown precipitate. The titration is repeated for concordant values.
7
Titration –II Determination of Chloride ions

20ml of the given water sample is pipette out into a clean conical flask and 1ml of 2% K2CrO4
indicator solution is added.It is then titrated against standardized AgNo3 solution taken in the burette.The
end point is the change of colour from yellow to reddish brown.The titration is repeated for concordant
values.

Titration –I Standardization of Silver nitrate

S.NO Volume of NaCl Burette Reading (ml) Concordant volume

(V1) ml Intial Final AgNo3 (V2) ml
1
2
3

Calculation of the normality of silver nitrate

Volume of sodium chloride V1 = 20ml

Normality of sodium chloride N1 = 0.1N

Volume of silver nitrate V2 = x

Normality of silver Nitrate N2 =

According to the law of volumetric analysis

V1N1 = V2N2

N2 = V1xN1/V2

= 20 x 0.1 /x

Normality of silver nitrate = --------- N

Titration –II Determination of Chloride ions

S.NO Burette Reading (ml)

8
 Volume of water sample Concardant volume of AgNO3
(ml) (ml)
1
2
3

Calculation

Volume of water sample V1 = 20 ml

Normality of water sample N1 =

Volume of silver nitrate V2 =

Normality of silver nitrate N2 =

According to the law of volumetric analysis

V1N1 = V2N2

N1 = V2 X N2/V1

Strength Of The Water Sample (N1) =

RESULT

Calculation of amount of the chloride

Amount of the chloride ion present in 1 liter = Eq.wt of chloride ion x strength of the chloride ion
(1000ml) of the water sample

= 35.46 x -------N

Amont of the chloride ions present in = --------------- x 100/1000

100 ml of the given water sample
= ---------------- x 1000 mgs

3. ESTIMATION OF HCl BY CONDUCTOMETRIC TITRATIONS

9
AIM:
To determine the neutralization point in an acid base titration using conductivity meter

REQUIREMENTS:
Conductivity bridge, Conductivity Cell, distilled water, 250ml beaker, stirrer, 0.1MHCl, 1.0 M NaOH

PRINCIPLE:
As the alkali is added from the burette into the cell containing acid, the concentration of H+ ions change
in a graphical manner, which leads to a considerable change in the electrical conductance of the solution,
which is measured using a conductivity meter. Then from the plot of conductance versus volume of
alkali, the precise neutralization point is determined. The titration of strong acid verses strong base
involves the following equation.

HCl + NaOH NaCl + H2O

In the titration of HCl against NaOH, initially the conductance of HCl solution is maximum due to
complete ionization. As the alkali is added, the conductance of solution decreases and after the
neutralization point the conductance starts increasing. This is because of the addition of the alkali. The
fast moving H+ ions are replaced by Na+ ions (slow moving) once the neutralization point is reached,
addition of alkali introduces fast moving OH- ions, there by increasing the conductivity of the solution.

PROCEDURE:
Pipette out 200ml of 0.1M HCl into a clean 250ml beaker. Fill the burette with 1.0M NaOH solution.
Dip a conductivity cell in the 0.1 M HCl solution and connect it to the conductivity meter and note the
initial conductance of solution. Run down the NaOH solution from the burette in small volumes of 1ml
and 0.5ml at the end point to be expected in to the cell and note the conductance.

OBSERVATION:

S.NO. Volume of NaOH (ml) Conductance (μs or mhos)

10
 1 0.5
2 1.0
3 1.5
4 2.0
5 2.5
6 3.0
7 3.5
8 4.0
9 4.5
10 5.0
11 5.5
12 6.0
13 6.5
14 7.0
15 7.5
16 8.0
17 8.5
18 9.0
19 9.5
20 10.0
21 10.5
22 11.0
23 11.5
24 12.0
25 12.5
26 13.0
27 13.5
28 14.0
29 14.5
30 15.0
31 15.5
32 16.0

GRAPH:

11
A plot of conductance on Y-axis versus volume of alkali on X-axis is drawn. Extrapolate the straight
lines and note the neutralization point of the graph.

Conductance
(mho)

Volume of NaOH (ml)

RESULT:

From the graph the volume of 1.0 M NaOH required for the neutralization of 0.1M HCl is
____________ml.

4. ESTIMATION OF ACETIC ACID BY CONDUCTOMETRIC TITRATIONS

12
 Aim
To determine the amount of acetic acid in the given solution using conduct metric titrations by strong
base

Requirements

Conductivity meter ,conductivity cell, distilled water 0.1M acetic acid,1.0M sodium hydroxide

Principle

Initially the conductance is low due to the feeble ionization of acetic acid. On the addition of base, there is
decrease in conductance not only due to the replacement of H+ by Na+ but also suppresses the dissociation
of acetic acid due to common ion acetate. But very soon, the conductance increases on adding NaOH as
NaOH neutralizes the un-dissociated CH3COOH to CH3COONa which is the strong electrolyte. This
increase in conductance continues raise up to the equivalence point. The graph near the equivalence point
is curved due the hydrolysis of salt CH3COONa. Beyond the equivalence point, conductance increases
more rapidly with the addition of NaOH due to the highly conducting OH − ions

Procedure
Pipette out 50 ml of 01.M acetic acid into a clean 250 ml beaker. Fill the burette with 0.1MNaOH solution.
Dip a conductivity cell in the 0.1M acetic acid solution and connect it to the conductivity meter and note
the initial conductance of a solution .Run down the NaOH solution from the burette in small volumes of
1ml at the end point to be expected in to the cell and note the conductance.

Tabulation
13
 S.No Volume of NaoH (ml) Conductance in mho
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15

GRAPH

Calculation

14
 Volume of NaoH consumed v1 = X ml

Normality of NaoH taken N1 = 1.0M

Volume of acetic acid V2 = 50 ml

Normality of acetic acid N2 = ?

Amount of acetic acid in the given solution = N2 X eq.wt of acetic acid

Result

Amount of acetic acid present in the given solution = gms

5. ESTIMATION OF HCl BY POTENTIOMETRIC TITRATIONS

15
AIM:
To determine the equivalence point between strong acid and strong base and to determine the normality of
HCl by titrating with NaOH using potentiometer.
REQUIREMENTS:
Potentiometer bride, standard cell, saturated calomel electrode, platinum electrode, quinhydrone, beaker,
burette, stirrer, 0.1NHCl, 1N NaOH, distilled water.
PRINCIPLE:
When a solution of strong acid (HCl) is titrated with the solution of a strong base (NaOH), the change in
PH will be reflected in the change in EMF. When a small amount of alkali is added to the acid, a little
change in the EMF is produced in the beginning. This change in electrode potential depends upon the
fraction of hydrogen ions removed. As an equivalence point reaches, the fraction of the hydrogen ions
removed by constant volume of standard alkali increases rapidly, there by causing a rapid change in the
EMF. Thus if the EMF of the cell is plotted against the volume of the standard alkali added, a curve is
obtained. As the changes in EMF is much more rapid near the equivalent point, the exact equivalent point
is obtained by differential method where, a graph of ΔE/ΔV vs volume of alkali added, gives the maximum
of the curve which corresponds to equivalence point of the titration.

HCl + NaOH NaCl + H2O

The cell can be represented as
H2(Pt)/ acid solution // KCl (aq) / Calomel electrode
PROCEDURE:
Pipette out 10ml of 0.1N HCl solution into 100ml beaker and saturate it with quinhydrone and dip the
indicator electrode (platinum electrode), connect the indicator electrode and saturated calomel electrode
(reference electrode) to the potentiometer. The two half cells are connected by means of a salt bridge. The
potentiometer is standardized and the used for measuring the emf directly. 1N NaOH is taken in the burette
and is added to the HCl solution.
Measure the emf of the acid taken in the beaker initially. First carry out the rough titrations by adding 1ml
of NaOH and measure the emf for each addition. The emf decrease gradually and then shows a sudden
decrease in the emf. Take enough readings after the sudden decrease in emf. From these rough titrations,
the range of end point is determined.
16
After finding the end point range, fair titrations are carried out by repeatedly adding 1ml of NaOH as before
and near the end point, small additions in the form of 0.1ml is added and emf is measured for each addition
and the readings are tabulated.
Graph is plotted with volume of alkali (NaOH) along X-axis and measured emf along Y-axis. A sigmoid
curve is obtained and the equivalence point is noted at the end point of intersection. To obtain a sharp end
point, another graph of volume of alkali (NaOH) along X-axis and ΔE/ΔV along Y-axis is plotted. The

maximum obtained in the curve gives the accurate equivalence point.

CALCULATION:

N1V1 = N2V2

Where, N1 = Strength of the acid

V1 = Volume of acid taken in the beaker
N2 =?
V2 = Volume of alkali from the graph.

Volume of NaOH (equivalence point) X Normality of NaOH

Normality of HCl =
2𝑎Volume of HCl taken (20ml)

= ………………….. N

17
OBSERVATION:
FAIR TITRATION:

Vol. of alkali (ml) EMF (mv) ∆E/∆V

0
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
8.1
8.2
8.3
8.4
8.5
8.6
8.7
8.8
8.9
9.0
9.5
10.0
11.0
12.0
13.0
14.0
15.0

RESULT:
The equivalence point of potentiometric titration between strong acid Vs strong base is
_______________ ml
The Normality of HCl by titrating with NaOH using potentiometer is ____________ N

18
 6. ESTIMATION OF FERROUS ION BY POTENTIOMETRY USING PERMANGANATE
Aim
To estimate the amount of ferrous ion in the given sample by potentiometry
Requirments
Beaker, potentiometer,burette, calomel electrode,platinum electrode,stirrer,Potassium
permanganate,ferrous sulphate, con.H2So4 ,distilled water
Principle
T he ferrous ion concentration in the given solution can be obtained by titration with standard potassium
permanganate by potentiometer. The combination of the saturated calomel electrode as reference electrode
and platinum electrode is used as indicator electrode.
10 FeSo4 +2KMno4 +8H2So4 ----------------------> K2So4+2MnSo4+5Fe2 (So4)3+8H2o
Procedure
Prepare 0.1N potassium permanganate solution by dissolving ------- gm of potassium permanaganate
in 1000ml of distilled water.Take 25ml of the ferrous solution into the beaker,add 25ml of 5N H2So4 and
50 ml of water.Fill the burette with potassium permanganate after rinsing the burette with potassium
permanganate.
Dip the saturated calomel electrode and bright platinum electrode. Set the stirrer in motion and measure
the initial EMF. Add 5 ml of permanganate to the beaker and measure the emf of the cell. After each
addition of potassium in 5 ml measure the emf of the cell. Determine the end point from the potential –
volume curve.

19
Tabulation & calculations:

S.No Volume of K2Cr2O7 (m) Emf (mv)

1 5
2 10
3 15
4 20
5 25
6 30
7 35
8 40

Volume of KMno4 from the curve = ‘x’ ml

Normality of KMnO4 = 0.1N

Volume of FeSo4 solution = 25 ml

Normality of Feso4 =

N1V1 = N2V2

N2 normality of FeSo4 = X* 0.1/25

Amount of FeSo4 = N2 x 55.85

= ------------------- gm/lit

Result

Amount of Ferrous ion present in the given sample = -------------------- gm/lit

20
7.DETERMINATION OF RATE CONSTANT OF ACID CATALYSED
HYDROLYSIS OF METHYL ACETATE
Aim
To determine the rate constant of hydrolysis of methyl acetate catalysed by an acid
Requirments
Burette,conical flask,iodination flask,plastic tray for thermostat,pipette,stop watch,water bath,Methyl
acetate, Hcl,NaoH,Phenolphthalien indicator
Principle
Methyl acetate is hydrolysed to give methyl alcohol, and acetic acid as shown below:
H+
CH3COOCH3+H2O ----------> CH3COOH+CH3OH

The reaction is catalyzed by hydrogen ions.In a dilute aqueous solution of the methyl acetate concentration
water being excess, is very high and practically remains constant during the reaction ,concentration of H+
which catalyse the reaction also remains constant .Thus the rate of reaction is dependent only on the
concentration of the methyl acetate, I.E.,
dx/dt =k[CH3COOH]
Following the kinetic equation of first order
K=20303/t log a/a-x
Since acetic acid is produced as a result of hydrolysis, the kinetics of reaction can be followed by
withdrawing affixed volume of the reaction mixture from time to time and titrating a standard alkali.The
titre value is equivalent to the some of the acid used as the catalyst ,which remains constant throughout
,and of the acetic acid produced during the reaction.The difference of titre values at any time after the
commencement of the reaction and that at the commencement gives the acetic acid formed and hence the
amount of methyl acetate hydrolyzed at that instant
Preparation of Reagents
1 .0.5MHCL: Dilute 4.3ml of 11.6N and 36% concentration Hcl (Mol.wt 36.5) to 100ml with distilled
water
2 .0.1M NaoH : Dissolve 0.4gms of NaoH (mol.wt 40 ) in 100 ml of distilled water.
3.Phnolphthalein Indicator: Dissolve 1gm of Phenolphthalein in 100 ml of distilled ethanol and add 100 ml
of distilled water with constant stirring, filter ,if necessary.
21
Procedure
1. Take 100 ml 0.5m Hcl in a dry 250ml conical flask and clamp it in the thermostat at 30c suspended
also a stoppered tube in thermostst and place in it about 15 ml methyl acetate.
2. Fill a burette with 0.1M NaoH solution ,previously rinsing it with the same solution.Take 3-4 conical
flask containnning about 250ml of ice cold water with small pieces of clean ice.
3. When temperature equilibrium has been reached pipette abot 5 ml of methyl acetate in to conical flask
containing ice cold water so to stop the reation.Record the time to the nearest 10 seconds when the pipette
has been half discharged in to the flask.Titrate this solution as rapidly with 0.1M NaoH using
phenolphthalein indicator.The titre value gives the amount of Hcl in the sample at the start of the reaction.
4. Make similar titration of further 5ml sample at successive intervals of 10,20,30,40,6,90 & 120 min.
5. Allow the remaining reaction mixture to stand for 48 hours so that reaction goes to completion.Titrate
5ml sample with alkali as before.If such as a long time is not available place the reaction vessel containing
the remaining reaction with its cork closed loosely ,in water bath at about 50ₒC for atleast 1hr to complete
the reaction.Then after cooling the flask to room temperature ,titrate 5ml of sample as before.Much time
can be saved if 25ml of the reaction mixture is placed in well stoppered small flask at about 50ₒC
immediately after taking the first reading .
As each molecule of ester is hydrolysed 1 molecule of acetic acid is produced .The acid concentration
,therefore increase as the reaction proceeds.This increase in acid conc.is a dieret measure of amount of
methyl acetate hydrolysis i.e, x If t0 & t∞ are titre readings at time Zero, t and infinitive the intial conc, a,
of the ester is proportional to the T∞-T0 and that time T.

Calculation

(a-x) to (T∞-Tt).The first order rate equationis a =T∞-To :(a-x) =T∞-Tt

k= 2.303/t log (T∞-To)/ (T∞-Tt)

t= 2.303 /k log (T∞-To) – log (T∞-Tt)

Graph Slope = y2-y1/x2-x1 = S value

22
Tabulation

Time in min Titre reading (ml) X ml (a-x)ml Log (a-x) k

Result:

The rate constant of the reaction (k) = ____________________________________

8a. SYNTHESIS OF ASPIRIN

23
Aim: To prepare aspirin from salicylic acid and acetic anhydride in presence of conc.H2SO4
Requirments: Salicylic acid = 5g or 2.5 g; Acetic anhydride, Con. H2SO4, Conical flask; Beaker; Buchner
funnel; Glass rod
Principle: Salicylic acid upon acetylation yields acetyl salicylic acid (aspirin). Acetylation proceeds
rapidly with acetic anhydride in presence of conc. H2SO4 as catalyst

Procedure:
Take 5 g of salicylic acid and 7 ml of acetic anhydride in a 100 ml conical flask. Add 3 drop of conc.
H2SO4 and shake well. Heat the flask on water bath keeping temp below 60-70oC for about 20 min. Cool
the mixture in an ice bath with stirring, then add about 20 ml of ice cold water to decompose excess of acetic
anhydride. Pour the contents of the conical flask into a 250 ml beaker containing 50 g of crushed ice. Stir it
until white solid appears. If white solid does not appear, scratch the sides of the flask with a glass rod or
stainless steel spatula, filter through buchner funnel and dry by pressing into the folds of filter paper.
Recrystallise the crude acetylsalicylic acid.
Recrystallisation:
Dissolve the solid in minimum amount of ethanol and dissolve it until clear solution is obtained. Clear solution
is allowed to cool slowly to get needle shaped crystals of Aspirin.
Calculations:
5 g X M . Wt of product
Theoretical yield =
M . Wt of starting material
Experimental value X 100
% Yield of Aspirin =
Theoretical value
Result:
The amount of Aspirin obtained = ……..g
The melting point of Aspirin =………oC

24
 8b.SYNTHESIS OF PARACETAMOL

Aim: To prepare Paracetamol 4-amino phenol and ethanoic anhydride

Requirements 4-amino phenol, ethanoic anhydride, Conical flask; magnetic stirrer, Buchner funnel,Bunsen
burner oven
Principle
4-aminophenol and ethanoic anhydride, are both IRRITANT's- avoid contact with hands or breathing in
vapours. If contact with skin or eyes wash with water: Paracetamol is dangerous in large quantities. Wear
safety glasses, gloves and lab coat

Procedure
Place 2g of the 4-aminophenol into a 50cm3 conical flask, add 15cm3 of water and stir the suspension
vigorously (magnetic stirrer) for a few minutes.Add 2.2cm3 of ethanoic anhydride and continue stirring until
the suspension dissolves and a precipitate (Paracetamol) eventually forms.After 10 minutes filter the
precipitate (using a buchner funnel), washing with small amounts of cold, distilled water.After drying, the
crude product should be placed in a clean 100cm3 conical flask and recrystalised by heating until it just
dissolves in approximately 20cm3 of water.Cool the flask in ice until crystals of the purified paracetamol
appear.Filter the crystals under vacuum, dry in a warm oven and then record the melting point and compare
with standard paracetamol tablets (~170oC).Repeat recrystalisation process to achieve a more purer product
Recrystallisation:
Cool the flask in ice until crystals of the purified paracetamol appear.Filter the crystals under vacuum, dry in
a warm oven and then record the melting point and compare with standard paracetamol tablets (~170oC).
Calculations:

5 g X M . Wt of product
Theoretical yield =
M . Wt of starting material
Experimental value X 100
% Yield of Paracetamol =
Theoretical value
Result:
The amount of Paracetamol obtained = …g
The melting point Paracetamol=…………oC

25
 10. DETERMINATION OF ACID VALUE OF COCONUT OIL

AIM: To determine the acid value of coconut oil

REQUIRMENTS :
Conical flask, water bath, burette, pipette, N/10 KOH, Neutral ethyl alcohol, phenolphthalein indicator ,coconut oil.
PRINCIPLE:
The acid value of lubricating oil is defined as the number of milligrams of potassium hydroxide required to neutralize
the free acid present in 1 gm of the oil.
The presence of mineral acids in lubricating oils is so rare that it is almost unnecessary to look for it, unless the oil is
refined in a faulty manner. In unused refined petroleum oils, the quantity is invariably negligible. When fatty acids are
present, or in the case of used oils, the acid content should be determined not because it gives any direct evidence of
corrosion hazard, but to sound a warning that a corrosion test might be revealing. In good lubricating oils, the acid
value should be very low. Increase in acid value should be taken as an indicator of oxidation of the oil which may lead
to gum and sludge formation besides corrosion. The acid value of fatty oils may vary from 0.2 to 50 and it shows the
extent of hydrolysis of glyceryl ester of the oil.
PROCEDURE :
Weigh out accurately about 5 gm of the oil under test into a 250ml conical flask and add 50 ml of neutral alcohol. Heat
the flask over a water bath for about 30 minutes. Cool the flask and the contents to room temperature and add a few
drops of phenolphthalein indicator. Titrate with the standard N/10 KOH solution until a faint permanent pink colour
appears at the end point.
C17H35COOH + KOH → C17H35COOK + H2O
Sometimes the pink colour at the end point may fade away after a little while due to the attack of alkali upon some
easily reachable material in the oil, particularly when the mixture is violently shaken. In such cases, the end point only
should be considered.

N
No. of ml of 10 KOH run down X 5.6
Acid value =
Weight of the oil taken in gm

Where 5.6 represents the amount of KOH in mg present per each ml of N/10 KOH solution (1000ml of 1N KOH =
56 gm of KOH)

RESULT

The given coconut oil has acid value =

26
11. VERIFICATION OF FREUNDLICH ADSORPTION ISOTHERM-ADSORPTION OF ACETIC
ACID ON CHARCOAL

AIM:
To study the adsorption of acetic acid on charcoal and verify Freundlich isotherm
REQUIRMENTS:
Stopped reagent bottles, burette, pipette, conical flask, beaker, charcoal, oxalic acid (0.25M) acetic acid,
(0.5M), NaOH (0.1 M), distilled water, phenolphthalein indicator.
PRINCIPLE:
The phenomenon in which accumulation of other substance on the surface of a porous
solid without a sensible penetration into the bilk of solid phase is called as adsorption.
At a given temperature, the variation in the amount of solute adsorbed with change
In concentration of the solution is given by an empirical relation suggested by Freundlich known as Freundlich
isotherm.
x/m = kc1/n
Where, x/m = amount of the absorbate adsorbed by mg of adsorbent
c = concentration of the adsorbent at a particular temperature k,n = empirical constants
Taking logarithms of the terms in freundlich isotherm we get

logx/m = logk + 1/n logc

The graph plotted between log x/m on Y-axis and log c on X-axis, a straight line will result. The slope of the
straight line will be equal to 1/n and the intercept gives logk

PROCEDURE:

Prepare 0.5 M acetic acid solution for 250 ml. With the help of two burettes add 10, 20, 30, 40, 50 ml of acetic
acid solution and 40, 30, 20, 10ml of distilled water in bottles 1, 2, 3, 4, 5, receptively.

Take the given unknown solution in the bottle no. 6. Mix the solutions well and keep all the six bottles in a
water bath for some time to acquire the temperature of the water bath. Weigh exactly 2 gms of activated
charcoal and add the same to each bottle. Shake the bottle well and keep in the water bath for about half an
hour. Prepare NaOH (0.1M) for 250ml and standardize with standard oxalic acid solution using
phenolphthalein indicator. Then determine the concentration of acid solution using standard NaOH solution.

Filter the solution of each bottle by means of filter paper. Collect the filtrates properly in flask. Reject first

27
few ml of filtrate in each case. Take 10 ml from each filtrate and then titrate with standard alkali. Calculate
equilibrium concentration of the acid in each bottle.
Tabulate the observations and result. Plot a graph between log x/m values and logCe values.

OBSERVATIONS ANDCALCULATIONS

Vol of M/10 NaOH Equilibrium

required for 10ml Initial concentration concentration of Amount adsorbed logC
Flask nos. x/m log x/m
solution of acetic acid, (Ci ) acetic acid x = Ci-Ce/20 e
after adsorption (Vml) ( Ce )

1
2
3
4
5

CALCULATIONS:

Amount of absorbent (charcaol) = 2 gms

Molarity of oxalic acid = M1

Molarity of NaOH = M2

V1M1 V2M2
=
n1 n2
28
V1 = Volume of oxalicacid M1 =

Molarity of oxalicacid

n1 = number of moles of oxalic acid reacted = 1

V2 = Volume of NaOH (titre value x ml)

n2 = number of moles of NaOH reacted = 2

V1M1 n2
M2 = X
n1 V2

V1M1 2
M2 = X
1 V2

Initial concentration of acetic acid in bottle no1

50
𝐶𝑖 = X M2
50
Concentration of acetic acid after adsorption in bottle no 1

2 x M2 x V
𝐶𝑒 =
50
First calculation the concentration (Ci) of acetic acid in moles/litre for each flask. From the titration data,
obtain the equilibrium value of Ce for each flask. The value of X for each can be calculated from the change
in concentration due to adsorption i.e.,(Ci – Ce ) and the initial volume of the solution (50 ml) as follows:

(Ci − Ce) 50 (Ci − Ce)

𝑥= = =
1000 20
From this, calculate the amount of acid adsorbed per gm of the adsorbent (x/m) in moles or in grams.

1. Plot a graph between log (x/m) values (ordinate) versus log Ce (abscissa). If the plot obtained
is a straight line, this will prove the validity of the Freundlich isotherm over the concentration range considered.
Evaluate the value of 1/n from the slope of the line and log K from the intercept on the ordinate by the straight line
for a value log Ce equal to zero.
RESULT:
The plot obtained is a straight line, so the Freundlich isotherm is verified _______.

29
 12. DETERMINATION OF VISCOSITY OF CASTOR OIL & GROUND NUT OIL BY
OSTWALD’S VISCOMETER

AIM
To determine the coefficient of viscosity of the given oil using Ostwald viscometer.
APPARATUS
Ostwald viscometer, 20ml. pipette, stop watch.
CHEMICALS
Oil, distilled water, acetone
PROCEDURE
Ostwalds viscometer is first cleaned with Chromic acid, then with distilled water and finally
rinsed with acetone. It is dried by passing hot air for some time. A rubber tube with pinch
cock is attached to the left hand limb. The viscometer is then clamped vertically to a retort
stand. A known volume of water usually about 20ml. depending upon the capacity of the bulb
D is pipette into the tube till it rises above the mark B. Then water is allowed to reflow through
the capillary tube under its own weight. When the water is just at B, the stop watch is started
and when it just passes the point C, the watch is stopped.The time required for the flow of the
liquid from B to C is noted.The above process is repeated 3 to 4 times and mean time (t1) of
flow is calculated.
Now the water from the viscometer is removed and then dried with Acetone. Then the time
required for the flow of same volume of oil from B to C is noted. After repeating the process 3 times the mean
time (t2) of flow is calculated.
We know
 𝑑1 𝑡1
=
 𝑑2 𝑡2

1 𝑑2 𝑡2
2 = 𝑑1 𝑡1

Where
1 = Coefficient of Viscosity of water
2 = Coefficient of Viscosity of the given liquid
d1 = Density of water
d2 = Density of the given liquid
t1 = Time taken for water
t2 = Time taken for the given liquid
Knowing all the values, the coefficient of viscosity of the oil is calculated.
30
 Observation Table:-

Time of flow of Organic liquid Viscosity (Centipoise)

Time of flow of water (Sec)  𝑑2 𝑡2
S.No. (Sec)
2 = 1
Trial – I Trial – II Average Trial – I Trial – II Average 𝑑1 𝑡1

Result

Viscosity of the given liquid is____________________centipoise

31
 13.DETERMINATION OF PARTITION CO-EFFICIENT OF ACETIC ACID BETWEEN n-
BUTANOL AND WATER.

AIM
To determine the partition co-efficeint value of acetic acid between n-butanol & water from the given solution
REQUIRMENTS: n-butanol, acetic acid, distilled water, NaOH Solution. Burette, pipette, 100 ml conical
flask, 250 ml Stoppered bottle, Wash bottle, Dropper
PRINCIPLE
Distribute between two immiscible solvents in contact with each other, then at equilibrium the ratio of the
concentration of the solute in two solvent layers is constant.
When a solute is shaken in two immiscible liquids, then the solute is found to be distributed between the
liquids in a definite manner, if the solute is soluble in each of the solvent.
According to distribution law, the distribution co-efficient at a particular temperature is given by
Kd = C1 / C2, where
C1 and C2 represent the concentration of solute in solvent 1 and 2 respectively. When the solute molecules in
each solution phase are in same state of association

PROCEDURE
i) A 250 ml stoppered bottle is taken and washed properly with distilled water.
ii) This bottle is filled up with 20 ml of n-butanol, 25 ml distilled water and 5 ml of acetic acid.
iii) Then it is allowed to shake in a mechanical shaker for about an hour. After shaking, it is kept aside for
about 5 minutes so that two layers separate out clearly.
iv) 5ml of aqueous layer is pipette out in a 100 ml conical flask. 2 -3 drops of phenolphthalein indicator is
added and titrated against standard NaOH solution until colour changes from colourless to pink.
v) 5ml of organic layer is pipette out in a 100 ml conical flask. 2 -3 drops of phenolphthalein indicator is added
and titrated against standard NaOH solution until color changes from colorless to pink.
vi) The experiments are repeated to get concordant values.

Tabulation

32
 Burette Reading Volume of
Pipette NaOH
Layers
Reading consumed Kd= C1 / C2
Taken Difference
(ml) Initial (ml) Final (ml) (ml)(Mean
(ml)
Vol.)(V)

Aqueous i)
Layer ii)

Organic i)
Layer ii)

Calculation:
Aqueous Layer (C1):
Volume of aqueous layer taken (V1) =
Volume of NaoH required (V2) =
Concentration of aqueous layer (N1) =
Concentration of NaoH layer (N2) =

Organic Layer (C2):

Volume of organic layer taken (V1) =
Volume of NaoH required (V2) =
Concentration of NaoH layer (N1) =
Concentration of organic layer (N2) =

Hence,
Kd = C1 / C2

Where C1 is the concentration of aqueous layer

C2 is the concentration of organic layer

RESULT:

Partition Coefficient of Acetic acid = between water & n-butanol

14.DETERMINATION OF SURFACE TENSION OF A GIVEN LIQUID USING

STALGANOMETER
33
AIM:
To determine the surface tension of a given liquid by using Stalagmometer.

REQUIRMENTS:.
Stalagmometer,. Specific gravity bottle, Rubber cork Analytical balance,Soap solution.. Methanol (or)
Ethanol

PRINCIPLE:
Surface tension is the characteristic properly of every liquid and it is due to intermolecular attraction among
molecules of liquid. A molecule in the interior part of the liquid is attracted by the surrounding molecules in all
directions and hence resultant force on the molecule is zero, whereas the molecules on the surface of the liquid
are attracted only towards the interior i.e., sides and the bottom are in constant tension due to the downwards
flow of the molecules in bulk, this tension at the surface is known as surface tension. It is defined as the force in
dynes acting on a surface at right angles to any line of unit length. It is denoted by “γ” (gamma) and its units are
dynes/cm.

Table given below lists the surface tension of several liquids at 200C.

Surface tension Surface tension

Liquid Liquid
(dynes/cm) (dynes/cm)

Water 72.8 Ethylene glycol 47.7

Benzene 28.9 Glycerol 63.4

Toluene 28.4 Carbon tetrachloride 27.0

Acetone 23.7 Ethyl iodide 29.9

Methyl alcohol 22.6 Ethyl bromide 24.2

Ethyl alcohol 22.3 Nitrobenzene 41.8

34
PROCEDURE

The determination of surface tension of a liquid involves the following 2 steps.

1. Determination of density of a liquid

Density of a liquid is mass/unit volume. It is found by using specific gravity bottles.

The specific gravity bottle is first washed with distilled water and finally with alcohol and dried. The weight of
the empty specific gravity bottle is found by using analytical balance. Let it be W1gm.Then it is filled with the
distilled water and its weight is accurately determined. Let it be W2 gm. Now the given unknown liquid is then
filled in the specific gravity bottles and the weight us found. Let this weight be W3 gm the density of the
unknown liquid (d2) is going to be calculated as:
Weight of liquid
Density of liquid (d2) = X density of water
Weight of the water

2. DETERMINATION OF SURFACE TENSION OF A GIVEN LIQUID:

The stalagmometer is first washed thoroughly with distilled water and finally with little alcohol and dried. A
clean rubber tube is attached to the upper end of the stalagmometer. A screw pitch cork is fixed on the rubber
tube to regulate the flow of liquid by lifting the influx of air.
The stalagmometer is dipped in a beaker of water and suck the water till it rises above the upper mark (X). In the
stalagmometer the water level is carefully brought to the mark (X). The pitch cork is opened in such a way that
it allows the flow of 12-18 drops per minute. Now the stalagmometer is adjusted.
Then water is sucked above the mark and the no of drops of water that flows from the mark (X) to the mark (Y)
are noted. This is repeated 3 to 4 times with water.
Now the stalagmometer is rinsed with the liquid whose surface tension is to be determined. The liquid is
then filled in the stalagmometer as above and no. of drops that flow from the mark (X) to mark (Y) is noted.
This is repeated 3 or 4 times with the liquid and the experimental results are noted in the tabular form.

35
CALCULATIONS
Calculation of density of the liquid Room temperature =27oC
Weight of empty specific gravity bottle (W1) =
Weight of specific gravity bottle + water (W2) =
Weight of specific gravity bottle + giveliquid (W3)=
Weight of water = (W2-W1) =
Weight of given liquid = (W3-W1) =
Density of water (d1) = 1 gm/cc
Weight of liquid
Density of liquid (d2) = X Density of the water
Weight of water

Volume of water
Concentration of Number of drops Surface
+ Volume of
S. No. soap/detergent tension
soap/detergent
solution Exp.1 Exp. 2 Average (N) (dynes/cm)
solution (ml)
1 50 + 0 Pure water
2 50 + 50 0.5%
Therefore the surface tension of given liquid (γ2) is determined busing the following equation.

n1d2
γ2= X γ1
n2d1
Where
γ 1 = Surface tension of water = 72.8 dynes/cm
n1 = no. of drops of water
d1 = density of water
γ 2 = surface tension of given liquid
n2 = no. of drops of given liquid
d2 = density of given liquid

Result
The surface tension of the given test liquid γ2 = …………… dyne/cm

36
 CONTENT BEYOND SYLLABUS
1. ESTIMATION OF FERROUS(Fe+2) IRON by DICHROMETRY
AIM:

To estimate the amount of ferrous iron in the given sample by using Potassium dichromate.

APPARATUS REQUIRED:

Conical Flask-250ml Weighing bottle

Burette-50ml Standard Flask-100ml

Pipette-20ml Funnel

Beaker-250ml

CHEMICALS REQUIRED:

Ferrous Salt Syrapy Phosphoric acid

Potassium dichromate Diphenylamine indicator

Conc.H2SO4 Distilled Water

Principle:

The ferrous iron present in the given sample reduced to Fe +3 iron by a standard K2Cr2O7 solution and
phosphoric acid & sulphuric acid 1:3 ratio. The end point is determined by colour change from deep
green to blue violet colour with the help of diphenylamine indicator.

Cr2O27 + 14H+ + 6Fe+2 → 2Cr+3 + 6Fe+3 + 7H2O

Procedure :

Step-I - Preparation of Standard K2Cr2O7 solution:

About 0.245 gms ofK2Cr2O7 is weighed out accurately and carefully transferred into a 100ml
standard flask with the help of a funnel and then the salt is dissolved in small amount of distilled
water and made upto the mark, slackened well for uniform concentration

The normality of K2Cr2O7 is determined.

37
Step – II – Estimation of ferrous iron in the given sample.

The given ferrous sample is made upto the 100ml mark with distilled water and shake well
for uniform concentration, the pipette is rinsed with the above solution and 20ml of the solution is
pipette out into a clean conical flask to this solution add about 10ml of acid mixture add 2 to 3
drops of Diphenylamine indicator. This solution is titrated with standard K2Cr2O7 taken in the burette
with constant shaking till the colour changes from light green to violet colour. The titration is
repeated till get concurrent values.

Calculations:

Step – I

 Weight of the empty bottle w1 = _________gms

 Weight of the empty bottle + salt w2 = _________gms
 Weight of the empty bottle + remaining salt (after transferring the salt) w3 =
_________gms.
 Weight of the salt (K2Cr2O7) = w2-w3 = _________gms.

Wt. of K2Cr2O7 (w2-w3) 1000

 Normality of K2Cr2O7 (N1)= ------------------------------ X --------
Eq.wt. of K2Cr2O7vml
(49)

= --------------------- N
Step 2:
S.No. Volume of Fe+2 Burette Values in (ml) Total value of
K2Cr2O7 (b-a) ml
Initial Final

N1 V1 = N2V2
N1 V1
N2 =
N1 = Normality of K2Cr2O7 V2
V1 = Volume of K2Cr2O7
N2 = Normality of Fe+2
V2 = Volume of Fe+2

Amount of ferrous ion present in the given 100ml solution is

38
 N2 x Eq. Wt of Fe(55.8)
=
10
Result: The amount of ferrous iron present in the given 100ml solution is _______ g

39
 2.Estimation of Ferrous and Ferric Ions in a given mixture by Dichrometry.

Aim:

To estimate the amount of ferrous and ferric ions in a given mixture by using potassium dichromate.

Required Apparatuas:

Burette Volumetric Flask

Pipette Weighing bottle

Conical Flask Beaker

Required Chemicals:

Pot dichromate stannous chloride

Mercuric Chloride Acid Mixture

Diphenylamine indicator

Principle:

During this estimation, total iron (Fe2+ + Fe3+) present in the sample is estimate by reducing
the Fe3+ to Fe2+ in presence of Sncl2. Then the same sample is estimated for the amount of
Fe+ presence and difference between the two values gives the amount of Ferric iron.

Total Iron (Fe2+ + Fe3+) – Fe2+ = Fe3+

2FeCl2 + SnCl2→ 2FeCl2 + SnCl4

SnCl2 + 2HgCl2→ Hg2Cl2 + Sncl4

K2Cr2O7 + 6 FeSO4 + 7H2SO4→ K2SO4 + Cr2(SO4) + 3Fe2(SO4)3 + 7H20

Procedure:

Step – I: Preparation of SD.K2CR207

Weigh accurately 0.245 of K2CR207 and prepare a standard solution in 100ml sd.flask using distilled
water. Shake the flask well for uniform concentration.

40
Step-II Standardisation of Ferrous iorn(Fe)

Pipetted 10ml of ferrous solution and 10ml ferric solution into conical flask added 5ml of acid
mixture and two drops of Diphenylamine indicator. Titrated against potassium dichromate. Taken
in burette till blue colour is obtained repeated the titration and noted the burette reading.

Step-III Standardisation of total iron mixture

Fill the burette with K2CR207 solution. Pipetted 10ml of ferrous solution and 10ml ferric solution into
conical flask and add 10ml of con. Hcl solution and heat the solution to boiling till the colour the
solution changes to clear yellow then add stannous chloride drop by drop to the hot solution till the
yellow colour disappears. Cool the solution under tap water and then add 10ml of mercuric chloride
solution till a silky white precipitate is obtained. Add 4ml of acid mixture and 3-4 drop of
Diphenylamine indicator and titrate solution against K 2CR207 taken in the burette till the colour
changes from green to blue violet.

Repeat the titration to get concurrent values. Let the titrate value be y ml.

Calculation:-

Step 1

 Weight of empty weighing bottle W1 = __________________

 Weight of weighing bottle + salt W2=___________________

 Weight of empty weighing bottle after transferring the salt W3= _________

 Weight of salt using for standard solution W2-W3 = ___________________

W2-W3 1000
Normality of K2CR207= --------- X -------
Mol.Wt100

N1 = --------- X 10 = __________________N
49

S.No. Volume of Burette Values in (ml) Volmue of

Ferrous K2CR207
solution Ml
ml
Initial Final

41
 1 20 0
2 20 0
3 20 0

Calculation:-

Step –II

Normality of Ferrous Solution (Fe2+) (N2)

V1 N1 = V2 N2

(K2CR207) (Fe2+Solution)

titre Value x N1 = 20 x N2

(x ml)

titre value X N1
N2 = --------------------
20

Amount of Fe2+ ion in 100ml for the given solution (P)

= N2 x 55.85 x 100
----- = _________________
1000

S.No. Volume of Burette Values in (ml) Volmue of

Ferrous K2CR207
solution Ml
ml
Initial Final
1 20 0
2 20 0
3 20 0

Calculation:-

Step –III

Normality of total iron mixture (N3)

42
N1 V1 = N3 V3

(K2CR207) (iron mixture)

N1 x titre value
N3 = --------------------
20

Amount of total mixture present in 100ml of given mixture (Q)

= N3 x 55.85 x 100
-----
1000

= _________________(Q) g.

Amount of Ferric Ion present in the given sample

= amt of Total Ion mix - amt of Fe2+

=Q-P

= _______g

Result :

The amount of Fe2+ ion present in the given sample (P) = _______________g
The amount of Fe3+ ion present in the given sample (Q) = _______________g

43
 VIVA QUESTIONS

Experiment: 1

.ESTIMATION OF HARDNESS OF WATER BY EDTA METHOD

1. What is hard water?

2. What do you mean by total hardness of water?
3. How is hardness in water classified?

4. What is the difference between temporary and permanent hardness?

5. What is EDTA?

6. What is a buffer solution?

7. What is the chemical name of Eriochrome Black –T?

8. How is temporary hardness removed?

9. How is the total hardness of water expressed?

10. Why is disodium salt of EDTA preferred to EDTA?

11. Why is ammonia-ammonium chloride buffer added?

12. Why is the indicator Eriochrome black –T (EBT) shows wine red colour at the

beginning and blue colour at the end of the titration?

13. Why are the titrations involving EDTA carried out slowly towards the end point?

44
 Experiment: 2

DETERMINATION OF CHLORIDE CONTENT OF WATER BY ARGENTOMETRY

1.What type of titration is chloride ion estimation?

2.What are the sources of chloride in water sample?
3.What are the reactions taking place in the estimation?
4. What is the product formed in this estimation?
5.What is the industrial importance of chloride ion estimation?

Experiment: 3&4

ESTIMATION OF AN HCL BY CONDUCTOMETRIC TITRATIONS &ESTIMATION OF ACETIC

ACID BY CONDUCTOMETRIC TITRATIONS

1. What is acid and base? Give examples.

2. What are weak electrolytes and strong electrolytes? Give examples.
3. When strong acid combines with strong base what type of reaction occurs?
4. Name the apparatus used for this method.
5. How conductance related to the concentration of the ions?
6. How the end point for a particular reaction is calculated using this, titration method?
7. Why conductance decreases on addition of NaOH to HCI ?
8. What is the unit for conductance?
9. What is the equivalent weight of HCI and NaOH?
10. Define conductometric titration.

Experiment: 5&6

45
 ESTIMATION OF HCL BY POTENTIOMETRIC TITRATIONS

ESTIMATION OF FE2+ BY POTENTIOMETRY USING KMNO4

1. What is potentiometric titration?

2. What is single electrode potential?
3. What is meant by emf?
4. What is potentiometer?
5. What is cell constant?
6. What are the electrodes used in potentiometric titration?
7. Explain the principle of potentiometric titration.
8. What is the determining factor in the oxidation-reduction reaction?
9. What is an indicator electrode ?
10. What are the advantages of potentiometric titration ?

Experiment: 7

DETERMINATION OF RATE CONSTANT OF ACID CATALYSED HYDROLYSIS OF METHYL ACETATE

1.What is chemical kinetics
2.What are the units of rate of reaction
3.what is thetemparature co-efficient of reaction
4.what are the units of the rate of reaction
5.what is first order reaction

Experiment: 8

SYNTHESIS OF ASPIRIN AND PARACETAMOL

1.why Aspirin is more soluble than Paracetamol

2.What are the different uses for aspirin?

3.What is the melting point of pure aspirin?

4.How do you purify aspirin?

5.How is aspirin synthesized?

6.How do you make aspirin?

46
 Experiment: 9

THIN LAYER CHROMATOGRAPHY CALCULATION OF RF VALUES. EG ORTHO

AND PARA NITRO PHENOLS
1.what is Rf value

2.what is the structure of ortho phenol

3.what is principle of TLC

4. what isrf value of ortho nitrophenol

Experiment: 10

.DETERMINATION OF ACID VALUE OF COCONUT OIL

1.What is the difference between acid value and saponification value?

2.What is acid value determination?

3.What is the acid value of castor oil?

4.What is the acid value of oil?

5.What is the unit of acid value?

6.What is iodine value of oil?

Experiment: 11

VERIFICATION OF FREUNDLICH ADSORPTION ISOTHERM-

ADSORPTION OF ACETIC ACID ON CHARCOAL

1.what is adsorption

2.what is adsorbent

47
3.what is absorption

4.what is adsorbate

Experiment: 12

DETERMINATION OF VISCOSITY OF CASTOR OIL AND GROUND NUT OIL BY USING

OSTWALD’S VISCOMETER.

1. What is Viscosity? Define surface tension.

2. How does the viscosity of a liquid vary with temperature?
3. What is specific gravity?
4. How are specific gravity and density related?
5. What is the S.I. unit of viscosity co-efficient and surface tension?
6. What is the significance of viscosity?
7. What is the meaning of volatile solvents?
8. What are the factors that influence the viscosity of a liquid?
9. What do you mean by all weather lubricants?
10. How is the viscosity of a liquid related to its mobility?

Experiment: 13

DETERMINATION OF PARTITION COEFFICIENT OF ACETIC ACID BETWEEN N-BUTANOL

AND WATER .

1.what is partition coefficient of liquid

2.what is the nature of acetic acid

Experiment: 14

DETERMINATION OF SURFACE TENSION OF A GIVE LIQUID USING STALAGMOMETER

1.What is the formula for surface tension?

2.What is a Stalagmometer?

48
3.What is Jaeger's method?

4.What is the capillary rise method?

CONTENT BEYOND SYLLABUS

Experiment 1.
ESTIMATION OF FERROUS IRON BY DICHOROMETRY
(Redox Titrations)

1. What is the redox reaction?

2. What is the oxidation number of ferrous iron?
3. What is an oxidizing agent?
4. What is reducing agent?
5. Define Normality and Molarity?
Experiment: 2

ESTIMATION OF FERROUS AND FERRIC IONS INA GIVEN MIXTURE BY

DICHROMETRY

1.What is the change of oxidation number of iron in the redox reaction?

2. What is the oxidation state of chromium in potassium dichromate solution?

3. Why is potassium ferricyanide cannot be used as an indicator in the estimation

of iron?

4. Why is the colour of the indicator drop remains the same at the end point?

5. Name the internal indicators used for iron determination?

6. What is the need of adding SnCl2 & HgCl2.

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