Eng - Chemsitry Labmanual

Engineering Chemistry Lab Manual (I B.
Tech Common to All)

Experiment-1
ESTIMATION OF HARDNESS OF WATER BY EDTA
(COMPLEXOMETRY)
Aim: To estimate the hardness of the given Sample water using a standard solution of EDTA.
Apparatus: 100 ml standard flask,

Burette,
250 ml Conical Flask,
20 ml Pipette,
& Simple balance with weights,
Chemicals Required: Ethylene di-amine tetra acetic acid (EDTA),

Solo-chrome (EBT) Indicator,
Ammonia Buffer solution,
Hard-water & distilled water.
Principle:
Hard water which contains calcium and magnesium ions forms a wine red colored complex
with the indicator, Eriochrome Black-T.
Ethylene diamine tetra acetic acid (EDTA) forms a colourless stable complex with free metal
ion like Ca, Mg. i.e., Metal + Indicator  Metal indicator complex (wine red colour)
When EDTA is added from the burette, it extracts the metal ions from the metal ion-indicator complex
thereby releasing the free indicator. (The stability of metal ion-indicator complex is less than that of
the metal ion- EDTA complex, and hence EDTA extracts metal ion form the ion-indicator complex.)
EDTA + Metal indicator complex  Metal ion-EDTA + Indicator

(Wine red color) (Blue)
The reactions take place at a pH = 10 and the buffer is made by ammonium chloride and ammonium
solution.
Procedure:
Preparation of standard hard water:

Dissolve 0.1g or 100 mg of CaCO3 in minimum quantity of dil.HCl in 100 ml standard flask.
Makeup the solution up to mark with distilled water.
1 mL hard water solution = 1mg of CaCO3 equivalent hardness.
Standardization of EDTA solution:

Rinse and fill the burette with EDTA solution. Pipette out 20 mL of standard hard water in a
conical flask. Add 2-5 mL of buffer solution and 2 to 3 drops of EBT-indicator. Titrate with EDTA
solution till wine-red colour changes to clear blue. Let volume EDTA solution used be V1 mL.
Titration of Unknown Hard water:

Rinse and fill the burette with EDTA solution. Pipette out 20 mL of Sample hard water in a
conical flask. Add 2-5 mL of buffer solution and 2 to 3 drops EBT-indicator. Titrate with EDTA
solution till wine-red colour changes to clear blue. Let volume of EDTA solution used be V2 mL.
__________________________________________________________________________________
Engineering Chemistry 1 SV GROUP OF INSTITUTIONS
Engineering Chemistry Lab Manual (I B.Tech Common to All)
Titration of Permanent hardness:

Take 200 mL of the water sample in a large beaker. Boil it. Till the volume is reduced to about
50 to 100 mL, filter it, collecting filtrate in a 100 mL standard flask, makeup the volume to 100 mL
with distilled water.
Rinse and fill the burette with EDTA solution. Pipette out 20 mL of Boiled hard water in a
conical flask. Add 2-5 mL of buffer solution and 2 to 3 drops EBT-indicator. Titrate with EDTA
solution till wine-red colour changes to clear blue. Let volume EDTA solution used by V3 mL.
Preparation of Standard hard water solution:
W1 = Weight of bottle + substance = ____________ gms
W2 = Weight of bottle = ____________ gms
Weight of substance = (W1-W2) = ____________ gms.
Titration of Standard hard water
S.No Volume of Standard Hard Burette Reading Volume of EDTA solution

water (Vs) Initial Final consume (V1)
1 20 ml
2 20 ml
3 20 ml
Vs = 20 ml V1 =
V1 =
(20 ml Standard hard-water reacting with 20 ml 0.01M EDTA solution)
Titration of Sample Hard water:

S.No Volume of Sample Hard Burette Reading Volume of EDTA solution
water (VH) Initial Final consume (V2)
1 20 ml
2 20 ml
3 20 ml
VH = 20 ml V2 =
__________________________________________________________________________________
V1 =
V2 =
Total hardness of water = 1000XV2

V1
Titration of Permanent hardwater
S.No Volume of Boiled Hard Burette Reading Volume of EDTA solution consume
water (VB) Initial Final (V3)
1 20 ml
2 20 ml
3 20 ml
VB = 20 ml V3 =
V1 =
V3 =
Permanent hardness = 1000 X V3

V1
Temporary hardness = 1000 X [(V2-V3)] =

V1
Result: The Temporary hardness of the given water sample _________ ppm.
The Permanent hardness of the given water sample ____ _____ ppm.
The Total hardness of the given water sample _____ ____ ppm.
__________________________________________________________________________________
Experiment-2
DETERMINATION OF PERCENTAGE OF COPPER IN BRASS
MINERAL ANALYSIS (IODOMETRY)
Aim: To determinate the percentage of Copper present in the given Brass sample using a standard
solution of Potassium Dichromate and Hypo as the link solution.

Funnel, Burette,
Iodometric flask,
Conical Flask,
20 ml Pipette & Simple balance with weights,
Chemicals Required: Brass sample,

Potassium Dichromate (K2Cr2O7),
Hypo (Na2S2O3),
Potassium Iodide (KI),
6N Conc.HNO3,
NaHCO3,
6N Sulphuric Acid (H2SO4),
Syrupy Phosphoric Acid (H3PO4),
Ammonia solution,
Potassiun thiocyanate (KSCN)
Starch & distilled water.
Principle:
Brass in an alloy which consists mostly of copper (60 to 80 %) and zinc ( 20 to 40% ) along
with small amounts of lead ( 0 to 2% ) , tin ( 0 to 6% ) and iron ( 0 to 1% ).
The experiment consists of dissolving a known quantity of brass in nitric acid, removing the
nitrate by fuming with sulfuric acid, adjusting the pH by ammonium hydroxide, complexion the iron
present using phosphoric acid, and finally titrating the copper ions with hypo by the iodo-metric
method.
When the brass sample is dissolved in nitric acid, the copper present is brought into solution in
the form of cupric ions. At the same time, tin is converted to meta-stannic acid
(SnO2.4H2O ), lead and zinc are oxidized to their respective soluble divalent ions, while iron is
converted to ferric ions. During the treatment with sulfuric acid, nitrate is eliminated, the meta-stannic
acid is re-dissolved and lead ions are precipitated as PbSO4 while all other metals go into solution as
their respective sulfates. Out of all the metal ions present in solution, only Cu 2+ and Fe3+ are reducible
by iodide. The interference by iron is eliminated by titrimetrically determined by the iodometric
method.
Chemical reactions:
2Cu2+ + 4I-  2CuI + I2
2S2O3 + I2  S4O6- + 2I-
Cu = I = S2O3-
__________________________________________________________________________________
Procedure:
1. Preparation of standard potassium dichromate:

Weigh out accurately about 0.490 gm or 490 mg of the given pure crystalline sample of
potassium dichromate and transfer into 100 ml standard (volumetric) flask. Dissolve the
dichromate in a small quantity of distilled water, and make upto the mark. Calculate the
normality of potassium dichromate.
2. Standardization of sodium thiosulphate:

Rinse the burette and fill it up with hypo. Pipette out 20 ml of potassium dichromate solution
and then transfer in to the conical flask and add 2 gm/spatula of sodium bicarbonate followed by
2 ml of concentrate HCl. Add 10 ml of 10%KI solution. Shake it well, stopper it, and keep it in
dark place for 5 minutes. Titrate the liberate iodine by running down hypo from the burette with
constant stirring upto 5 ml. When the solution attains a pale yellow colour add 2 ml of freshly
prepared starch solution. The colour changes to blue. Continue the titration drop-wise till the
colour changes from blue to light green indicating the end point.
3. Estimation of copper:
About 0.25 g or 250 mg of clean and dry brass sample is accurately weighed and
transferred into a conical flask. Add bout 10ml of 6 N HNO3 and the flask is gently heated
until the brass sample is completely dissolved. Then 10ml of conc. H 2SO4 added and the
solution is evaporated on a sand bath to copious white fumes. The mixture is then allowed to
cool and 20ml of water very carefully add from the sides of the flask, in installments of 1ml
at a time while cooling under a tap. Boil the solution for 2 minutes and cool. Add liquor
ammonia drop-wise while shaking the flask vigorously until the appearance of blue cupric
ammonium complex. Now, 6N H2SO4 is slowly added drop wise until the dark Blue colour
disaapears. Then add 2 ml of syrupy phosphoric acid. The solution is cooled and transferred
to a 100ml volumetric flask. The volume is made up to the 100ml mark using distilled water.
20 ml of this solution is pipette out into a 150ml conical flask and add about 1 g of solid (KI)
potassium iodide. The flask is shaken and the solution is immediately titrated with standard
sodium thio-sulphate solution until the solution assumes a faint yellow colour of iodine.
About 1 ml of 1% starch solution are added and the titration is continued until the blue colour
begins to fade. At this stage, about 0.5g or 500 mg of potassium thiocyanate (KCNS) is
added and the titration is continued until the blue colour just disappears. The titration is
repeated twice with fresh 25ml portions of the solution to confirm the titer value.
4. Weight of Brass Sample (B):
W1 = Weight of bottle + Brass sample = ____________ gms
Weight of Brass Sample = B = (W1-W2) = ____________ gms.
Weight of the Brass Sample = B =
__________________________________________________________________________________
5. Preparation of Standard (K2Cr2O7)solution:
Normality of the solution = (W1-W2) X 10__ = (W1-W2) X 10 =

Equivalent Weight 49
Standardization of sodium thiosulphate:
S.No Volume of standard Burette Reading Volume of

(K2Cr2O7)solution (V1) consume (V2)
Initial Final
1 20 ml
2 20 ml
3 20 ml
V1 = V2 =
N1 = Normality of Potassium dichromate =
V1 = volume of Potassium dichromate = 20 ml
N2 = Normality of Hypo =?
V2 = Volume of Hypo =
N1 V1 = N 2 V2
N2 = N1 V1 =
V2
N2 = Normality of Hypo =
__________________________________________________________________________________
ESTIMATION COPPER:
S.No Volume of Copper Burette Reading Volume of

solution (V3) consume (V4)
Initial Final
1 20 ml
2 20 ml
3 20 ml
V3 = 20 ml V4 =
N3= Normality of Copper solution = ?
V3 = volume of Copper Solution = 20 ml
N4 = Normality of Hypo =
V4 = Volume of Hypo =
N3 V3 = N 4 V4
Normality of Copper solution = N3= N4V4

V3
The amount of copper present in the solution can be calculated on the basis that
1ml of 1N Na2S2O3 = 0.06354 g of Cu.
Amount of Copper present in the whole of the given solution (100 ml) = Z = N3 X 63.54 X 1000
100
Weight of the Brass Sample = B =
Percentage of Cu in the brass sample : (% of Cu in brass) = Z X 100 =

B
Result: Percentage of Copper present in the whole of the given Brass sample(100 ml) = ______ %.
__________________________________________________________________________________
Experiment-3
ESTIMATION OF MANGANESE DIOXIDE IN PYROLUSITE.
MINERAL ANALYSIS
Aim: To estimate the amount of MnO2 present in the given sample and hence percentage purity of
Pyrolusite.

Burette,
Conical Flask,
20 ml Pipette,
Funnel,
Simple balance with weights,
Heating equipment.
Chemicals Required: Pyrolusite,

4N Sulphuric acid (H2SO4),
0.1 N Di Sodium oxalate solution,
Potassium permanganate (KMnO4),
Distilled water.
Principle:
The MnO2 present in the pyrolusite sample is reduced by a known excess of standard sodium
oxalate in acid medium. The unreacted sodium oxalate is titrated against a standard KMnO4, until pale
pink coloured end point is obtained.
MnO2 + H2SO4 + H2C2O4  2CO2 + 2H2O + MnSO4
1ml of 1N KMnO4 = 1 ml of 1N Na2C2O4 = 0.04346 gm of MnO2 = 0.01099 gm of Mn
1 ml of 1N KMnO4 = 1 ml of 1N As2O3 = 0.04346 gm of MnO2
Preparation of Standard Di-Sodium Oxalate solution:

Weigh accurately 0.67 gm of Di-Sodium Oxalate and transfer into 100 ml standard flask
through a funnel. Dissolve the compounds small amount of distilled water and make up to the mark
with distilled water. Shake the flask vigorously for uniform standard Di-Sodium Oxalate solution.
Standardization of KMnO4 solution:

Take 20 ml of the 0.1N sodium oxalate solution in a conical flask; add 50 ml of 4N H2SO4
solution. Titrate with the KMnO4 solution at room temperature until the faint pink colour appears.
Warm the solution to 60 to 700 C and continue the titration to a faint permanent pink colour.
Estimation of MnO2:
Weigh out accurately about 0.1 gm or 100 mg of the given powdered pyrolusite sample into a
clean dry conical flask and add 50 ml of standard sodium oxalate solution and add 50 ml of 4N
(H2SO4) sulphuric acid, put a small funnel into the mouth of the conical flask. Heat with small flame
till particles are MnO2 disappear in the conical flask. Rinse the funnel with distilled water into the
conical flask, titrate the hot solution, containing the unreacted sodium oxalate with standard KMnO 4
solution till there is a pale pink colour.
Result: Percentage purity of the given sample of Pyrolusite =
__________________________________________________________________________________
Preparation of Standard sodium oxalate solution:
Normality of the solution = (W1-W2) X 10 = __________X 10

Equivalent Weight 67
Standardization of KMnO4 solution:

S.No Volume of standard Burette Reading Volume of
di sodium oxalate KMnO4consume (V2)
solution (V1 ) Initial Final
1 20 ml
2 20 ml
3 20 ml
V1= 20 ml V2 =
N1 = Normality of di sodium oxalate =
V1 = volume of di sodium oxalate = 20 ml
N2 = Normality of KMnO4 =?
V2 = Volume of KMnO4 =
N1 V1 = N 2 V2
N2 = N1 V1 =
V2
N2 = Normality of KMnO4 =
__________________________________________________________________________________
Weight Of the Pyrolusite Sample:
W1 = Weight of bottle + Pyrolusite = ____________ gms
Weight of Pyrolusite = (W1-W2) = ____________ gms.
S.No Volume of standard Burette Reading Volume of consume

solution (V)
Initial Final
1 50 ml
2 50 ml
3 50 ml
V=
Calculations:
Weight of the Ore taken =
Volume of 0.1N Di sodium oxalate solution added in the experiment = 50 ml
Volume of 0.1N KMnO4 run down = V =
Volume of 0.1N KMnO4 consumed = (50 – V) =
1 ml of 1N KMnO4 = 1N Na2C2O2 = 0.04346 g of MnO2
Percentage of MnO2 = (50 - V) X Normality of KMnO4 X 0.04346 X 100

Weight of the sample
Result: Percentage purity of the given sample of Pyrolusite =

__________________________________________________________________________________
Experiment-4
DETERMINATION OF FERRIC IRON IN CEMENT BY COLORIMETRIC METHOD
(Colorimetric Estimation)
Aim: To estimate the amount of Iron (Ferric) present in a sample of cement by calorimetrically using
ammonium thiocyanate as a reagent.
Apparatus: 250 ml beaker,

Glass rod,
Watch glass,
100 ml standard flask,
Burette,
10 ml Pipette,
Simple balance with weights
Colori-meter,
Heating-equipment.
Chemicals Required: Cement sample,

Conc. Nitric acid (HNO3),
Hydrochloric acid (HCl)
Ammonium thio-cyanate &
Distilled-water.
Principle:
Ammonium thio-cyanate yields a blood red colour with ferric iron and the colour produced is
stable in nitric acid medium. Its optical density is measured in a photo colorimeter and the
concentration of ferric iron is found from a standard calibration curve.
Procedure:
1. Dissolution of the sample:
Weight out accurately about 0.1 gram or 100mg of the cement sample into a clean 100 ml
beaker add about 5 ml of water to moisten the sample, add about 5 ml conc. Hydrochloric acid
(HCl) drop-wise and heat the solution till the sample dissolved. Keep the beaker on a small flame
and evaporate the solution to almost dryness to expel the excess acid.
Take the beaker out of the flame and add about 20 ml distilled H2O to dissolve the contents.
Transfer the solution into 100 ml standard flask. Wash the beaker twice with small portions of
distilled water, and add the washings to the standard flask. Make up the solution to 100 ml with
distilled water. Shake the flask well uniform concentration.
__________________________________________________________________________________
2. Development of Colour:
Pipette out 10 ml of the solution prepared above, into a 100 ml standard flask; add 1 ml of
conc. Nitric acid (HNO3) and 5 ml of 40% ammonium thiocyanate. Make up the solution to 100 ml
with distilled water and shake the flask well for uniform concentration. Find out the optical density
of the solution using the photo colorimeter and the concentration of the ferric iron from the
calibration curve.
Result: Percentage of Ferric iron present in the cement sample =
Weight of the sample:
W1 = Weight of bottle + sample = ____________ gms
Weight of sample = (W1-W2) = ____________ gms. = ___________ mg
Standard value for calibration curve
Concentration in Milligrams O. D
0.01 0.03
0.02 0.05
0.03 0.07
0.04 0.09
0.05 0.11
0.06 0.13
0.07 0.15
0.08 0.17
0.09 0.19
0.10 0.22
0.11 0.24
0.12 0.26
__________________________________________________________________________________
0.13 0.28
0.14 0.30
0.15 0.32
0.16 0.34
0.17 0.35
0.18 0.37
0.19 0.39
0.20 0.40
0.21 0.42
0.22 0.44
0.23 0.46
0.24 0.48
0.25 0.50
0.30 0.62
0.35 0.70
0.40 0.80
Optical density of given sample solution = O.D =
Corresponding amount of ferric iron from the calibration curve = X = ________ mg.
Calculation:
Percentage of Fe3+ present in the given cement sample = X x 10 x 100

(W 1 – W2) mg
Result: Percentage of Ferric iron present in the cement sample =
__________________________________________________________________________________
Experiment-5
CONDUCTOMETRIC TITRATION OF STRONG ACID Vs STRONG BASE
(CONDUCTOMETRY)
Aim: To estimate the amount of HCl present in given solution.
Apparatus:
Conductivity meter,
Conductivity cell,
Burette,
Pipettes,
Beakers &
Stirrer.
Chemicals Required:
Pure sample of Oxalic acid,

0.02M HCl and
0.1M NaOH.
Theory:
Electrolytic conductivity is a measure of the ability of a solution to carry electric current.
Solutions of electrolytes conduct electric current by the migration of ions under the influence of
applied field. Like metallic conductors they obey ohms law. At a given temperature the conductivity
depends upon the concentration of the electrolyte.
Conductivity cell:
The electrolytic conductance of an electrolyte is measured in conductivity cells, which are

specially designed. These are available in various sizes and shapes consisting of 2 electrodes. Each
electrode is a pH disc or plate coated with finely divided Pt black. The electrode is welded to a Pt wire
which is fused to a glass tube. The glass tubes are firmly fixed in the cell so that the distance between
the electrodes would not change during the experiment. The cell is open at one end; the electrolyte
whose conductivity is to be measured is dissolved in water and is taken in a beaker. The conductivity
cell is placed in the solution and is connected to the conductometer.
Cell constant X:
X of a conductivity cell is the ratio of distance between the 2 electrodes and the exposed area
of one of the electrodes.
X=1
a
Specific conductance:
It is the conductance of ions present in one cubic centimeter of the solution. If the cell constant
of a conductivity cell is 1.0 the measured conductivity of an electrolyte is its specific conductivity. The
cell constant of a conductivity cell is seldom 1.0 cm-1, also measuring ‘l ‘and ‘a ‘are troublesome.
Hence the given cell is calibrated for its cell constant, with the help of an electrolytic solution
normally, a standard KCl whose specific conductivity is known.
Cell constant = known specific conductance / measured conductance

__________________________________________________________________________________
Principle:
The electrical conductance of an electrolytic solution is proportional to a) the ionic

concentration i.e. number of ions present in the solution and b) the ionic mobilies. The ionic motilities
in aqueous solutions are generally of the order of 6.0 x 10-4 cm2, sec-1 volt-1. But the ionic mobilities
of H+ and OH- are abnormally high, H+ = 36.3 x 10-4 and OH- = 20.5 x 10-4 cm2 sec-1 volt-1. Thus the
conductance of an electrolyte is quite sensitive to concentration of H+ and OH- ions.
Titration of strong acid HCl with strong base NaOH:
In solution HCl is completely ionized. The mobility of H+ ions is high; hence the conductance
of HCl solution will also be high. As NaOH is added to HCl, the fast moving H + ions are removed by
OH- ions of the base as water.
H3O+ + OH- = 2H2O
In solution water is little ionised and Na+ added are slow moving compared to H+ ions of acid. Hence
as the titration proceeds, the conductance of titrand HCl decreases gradually till the equivalent point is
reached. At the equivalence point the conductance of the solution will be the minimum addition of the
base beyond end point adds Na+ and fast moving OH- ions, resulting in a gradual increase in
conductance.
PROCEDURE:
Preparation of Standard Oxalic acid solution:
Weigh accurately 0.630 gm or 630 mg of Oxalic acid and transfer into 100 ml standard flask
with distilled water. Shake the flask vigorously for uniform standard Oxalic acid solution.
Standardization of NaOH solution:
Pipette out 20 ml of prepared NaOH solution in a conical flask. Add 1-2 drops of methyl
orange indicator and titrate against standard oxalic acid solution.
Determination of Cell constant:
Take a conductivity cell and determine its cell constant using a 0.1 N KCl solution.
Conduct metric titration:

The burette is rinsed and filled with 0.1 M NaOH, 40 ml of given acid is placed in a 100 ml
beaker. The cell is washed with conductivity water which is placed in HCl solution and see that the
electrodes of cell are completely immersed in the solution. The cell is fixed in a cell holder and is
connected to the conductivity bridge. The conductance of HCl solution is noted at a time when 1 ml of
NaOH from the burette is added into HCl solution. After each addition the solution is stirred gently
with a glass rod and the conductance of HCl is noted. The titration is continued till 20 to 25 ml of
NaOH is added.
Graph:
Plot a graph between the conductances measured on Y-Axis and volume of alkali added (X-
Axis) we get a V shaped graph the point of intersecting will be the End-Point of titration and will
determines the volume of alkali required for neutralization of the acid.
__________________________________________________________________________________
CALCULATIONS:

Equivalent Weight 63.03
S.No Volume of standard oxalic acid Burette Reading Volume of NaOH

solution (V1 ) consume (V2)
Initial Final
1 20 ml
2 20 ml
3 20ml
V1 = V2 =
N1 = Normality of Oxalic acid =
V1 = volume of Oxalic acid = 20 ml
N2 = Normality of NaOH =?
V2 = Volume of NaOH =
N1 V1 = N 2 V2
N2 = N1 V1 =
V2
N2 = Normality of NaOH =
__________________________________________________________________________________
S.No Volume of NaOH solution added (ml) Conductivity of the solution (ohm-1)
1 0.0
2 1.0
3 2.0
4 3.0
5 4.0
6 5.0
7 6.0
8 7.0
9 8.0
10 9.0
11 10.0
12 11.0
13 12.0
14 13.0
15 14.0
16 15.0
17 16.0
18 17.0
19 18.0
20 19.0
21 20.0
22 21.0
23 22.0
24 23.0
25 24.0
26 25.0
__________________________________________________________________________________
Volume of the Hydrochloric acid (HCl) used = 40 ml
Volume of NaOH required to reach Equivalent Point = V =
Normality of NaOH =
Strength of HCl = End point titer valve (V) X Normality of NaOH =

Volume of HCl used
Result: The strength of HCl calculated is __________ N.
__________________________________________________________________________________
Experiment-6
TITRATION OF STRONG ACID VS STRONG BASE BY POTENTIOMETRY
(POTENTIOMETRY)
Aim: To estimate the amount of HCl present in given solution.
Apparatus: Saturated calomel electrode,

Platinum electrode,
Quinhydrone electrode,
Potentiometer,
Salt bridge,
Burette,
Pipette,
Beakers & glass rod etc.
Chemicals Required: Pure sample of Oxalic acid,

0.1M HCl and 0.1M NaOH.
Principle:
Quinhydrone (Q) is an equi-molar mixture of quinine C6H4O2 and Hydroquinone C6H4(OH)2.
In acidic medium the following redox equilibrium is established.
Q +2H+ + 2e- ↔ QH2
A pinch of quinhydrone added to an acid solution and a Pt wire or foil dipped in it constitutes a half
cell such electrodes are called indicator electrodes. This is coupled with a reference electrode through
a salt bridge making it an electrochemical cell.
Ex:(-)saturated calomel electrode / salt bridge / Qunihydrone + Acid solution / Pt +

(or)
(-) Pt, Hg / Hg2Cl2 (s) / KCl (saturated) // H+ , QH2, Q/Pt (+)
CELL REACTION:
2 Hg(s) + Q + 2Cl-(aq) ↔ Hg2Cl2(s) + QH2
Ecell = Eright – Eleft in terms of reduction potentials
Ecell = EQE – 0.242 ---------(1)
The left hand half cell is fixed i.e., its potential is constant. Now the right hand half cells potential
depends on H+ activity. The fundamental equation governing the effect of activity of the ions on the
voltage of an electrode or a cell is Nernst equation given by
Ecell = Ecell - (RT / nF ) lnk

Where k is equilibrium constant of a general reaction aA + bB ↔ cC + dD
The potential will be EQE + nE0QE – (RT /2F ) ln (QH2) / (Q) (H+)2
EQE = E0QE + 0.0591 log (H+) – 0.242
Ecell = 0.458 – 0.0591 pH

__________________________________________________________________________________
During the titration, against and alkali, H+ ion concentration in the half cell containing QH2
will decrease correspondingly the Ecell decreases. The emf will change slowly in the beginning how
ever at the end point relatively higher potential difference will be obtained and then again it will
change slowly. After the end point 5 or 6ml more of the bas is added, quickly and EMF is recorded.
Repetition of titration is done by adding 0.2ml of Na OH at a time near the end point. A graph is
plotted between EMF and volume of base added. The point of inflection where the graph changes its
direction is the end point. A differential plot of (E/V) against V* give s a curve whose peak
indicates equivalent point.
PROCEDURE:
Weigh accurately 0.630 gm or 630 mg of Oxalic acid and transfer into 100 ml standard flask
with distilled water. Shake the flask vigorously for uniform standard Oxalic acid solution.
Pipette out 20 ml of prepared NaOH solution in a conical flask. Add 1-2 drops of methyl
orange indicator and titrate against standard oxalic acid solution.
INSTRUMENTATION PROCEDURE:
1) Calibrate the instrument before starting the experiment.

2) Take 20 ml of acid solution in a 100 ml beaker and immerse the pH electrode in to the solution.
3) Firist carry out the rough titrations by adding 1 ml of NaOH and measure the EMF at each
stage.
4) After finding the range of end point, then take fresh sample of acid solutions in a beaker and
carry our the titrations repeatedly by adding 5 ml, 3ml, 2ml, 0.5ml, 0.2ml and 0.1ml
successively.
5) After the end point, the volume of alkaline added is increased to 1 or 2 ml. Near the end point
smaller addition should be added by micro burette.
6) Plot pH values or EMF values against the volume of NaOH added. Draw a smooth curve, the
point of intersection gives the equivalence point.
7) Plot another graph between E / V values against the titre readings abscissa. The maximum
of the curve represents the equivalence point.
Graph:
Plot a graph between cell EMF on Y-Axis and Volume of NaOH on X-Axis. For getting the
exact neutralization point another graph drawn E/V Vs Volume of NaOH from this graph the
volume required for neutralization is known.
__________________________________________________________________________________
__________________________________________________________________________________

Equivalent Weight 63.03
S.No Volume of standard Burette Reading Volume of NaOH

oxalic acid solution consume (V2)
(V1 )
Initial Final
1 20 ml
2 20 ml
3 20 ml
V1= 20 ml V2 =
N1 = Normality of Oxalic acid =
V1 = volume of Oxalic acid = 20 ml
N2 = Normality of NaOH =?
V2 = Volume of NaOH =
N1 V1 = N 2 V2
N2 = N1 V1 =
V2
N2 = Normality of NaOH =
__________________________________________________________________________________
TABULER FORM:
S.No Volume of NaOH EMF value (mv) E V E/V
(ml)
1 0
2 1
3 2
4 3
5 4
6 5
7 6
8 7
9 8
10 9
11 10
12 11
13 12
14 13
15 14
16 15
17 16
18 17
19 18
20 19
21 20
22 21
23 22
24 23
25 24
26 25
Volume of NaOH (Eqv.point) =
Normality of NaOH = N2 =
Volume of HCl taken =
Normality of HCl = volume of NaOH (Eqv.point) X Normality of NaOH

Volume of HCl taken
RESULT: the normality of HCl by titrating with NaOH using potentiometer is ________ N .
__________________________________________________________________________________
Experiment-7
DETERMINATION OF VISCOSITY OF SAMPLE OIL BY REDWOOD VISCOMETER.
OBJECTIVE:-
1. To determine the Absolute and Kinematic Viscosities of a given sample of oil at various
temperatures starting from room temperature.
2. To draw the following graphs.
 Absolute viscosity Vs Temperature.
 Kinematics Viscosity Vs Temperature.
APPARATUS:-
Red wood Viscometer-I,
Thermometers 2No. (0--1100),
Stop watch,
Measuring flask (50ml),
Energy regulator and sample oil.
THEORY:-
Viscosity is one of the important properties of a lubricant, which helps in selection of
oils for their suitability for lubricating purposes. A lubricant when used is aimed at reducing friction
between different moving parts of a machine by avoiding direct metal-to-metal contact. The thin film
of oil, formed between the moving surfaces, keeps them apart and thus the frictional resistance is
entirely on account of the shearing of the liquid. The viscosity of the fluid measures the amount of the
internal friction.
The objective of this experiment is determining the viscosities, therefore, is to ascertain
whether the oil is sufficiently viscous, under the high pressure and temperature conditions of the
machine, to adhere to the bearing. The variation of viscosity with temperature is of great importance to
the engineer in all problems of fluid flow and fluid friction and also in pumps, fans and all types of
bearings.
Absolute Viscosity:-
It is the shear force required to move a layer of the oil of one-centimeter thickness over
an area of one square centimeter thickness. In C.G.S system it is expressed in poise and in SI system it
is expressed in 1N-Sec/m2
1N-Sec/m2 = 10 poise; dyne-sec/cm2=poise
Kinematic Viscosity:-
The ratio of Absolute Viscosity to the density is called Kinematic Viscosity. In C.G.S
system it is expressed in Stokes and in SI system it is expressed in m2/sec
1m2/sec = 104 stokes; stoke = cm2/sec
Effect of temperature on Viscosity:

Increase in temperature causes a decrease in the viscosity of a liquid; where as viscosity
of gases increase with temperature the viscous forces in a fluid are the outcome of inter molecular
cohesion and molecular momentum transfer. In liquids the molecules are comparatively more closely
packed, molecular activity is rather small and so the viscosity is primarily due to molecular cohesion.
__________________________________________________________________________________
Since the rate, at which a fluid will flow through an aperture, increase as the internal friction of
the fluid decreases, the rate of flow through an orifice or short tube may be used as a means for
measuring viscosity. This is the principal involved in Redwood Viscometer-I, which is used in United
Kingdom for measuring viscosity. The time in seconds required for 50ml of oil to gravitate through the
Redwood Viscometer at a given temperature is expressed as its viscosity in Redwood seconds at that
temperature. The Kinematic and Absolute viscosities can be determined from Redwood seconds by
using the following formulae
Kinematic Viscosity (υ) = At – B/t
Absolute Viscosity (µ) = υ.ρ
Where A and B are constants, t is Redwood seconds and ρ is the density of the fluid.
Redwood Viscometer-I is used for determining the viscosity for low viscosity oils. It has an
orifice of diameter 1.62 mm with a length of jet of 10mm. The values of A and B for Redwood
Viscometer-I are as follows
Viscosity range in R.I A B

seconds
40-85 0. 264 190
85 to 2000 0. 247 65
DESCRIPTION OF APPARATUS:
The Redwood Viscometer consists of a heavily silver plated oil cup with a dish
shaped bottom with a standard hole in hemispherical seating. A spherical ball valve is placed to close
the orifice. The oil cup is surrounded by a bright chrome plated water bath. The water bath is mounted
on a stand with leveling screws. The level to which the oil is to be filled into the cup is given by an
index fixed to the inside wall of the oil cup. A standard size stainless steel jet is fitted at the center of
the bottom of the cup for the flow of oil to be measured. The cylindrical water bath is provided with a
tap for emptying. The water bath surrounding the oil cup provided with three vanes, having their upper
and lower positions rotated in opposite directions to facilitate stirring, which is carried out manually.
For ascertaining the level of equipment a flat circular spirit level is used. The
flow of oil is regulated by the ball value.
The oil cup cover is fitted with an insulated handle, and has suitable
arrangement to facilitate thermometer and value rod. The circular spirit level is mounted on a plate to
fit on the upper end of the oil cup.
PROCEDURE:-
i. Clean the oil cup and dry it. Examine the jet and ensure that it is clean and not obstructed.
ii. Mount the bath on the stand and level it with the help of spirit level and leveling screws.
iii. Fill the water bath with water until the heating element is below the water surface. Fill the oil
cup with oil up to the mark.
iv. Fix the thermometers in the provided space intended for measuring water and oil temperatures.
v. Press the connector to the water bath heater pin and the three-pin plug to the plugged to the
socket of the energy regulator box. The three-pin plug from the energy regulator is connected
__________________________________________________________________________________
to the socket of the main supply. Keep the energy regulator knob at the eighty marks and
switch ON the main supply.
vi. Water gets heated and the water temperature reaches 600C stir them well and ensure that the
water and oil temperature are nearly equal.
vii. Place the clear dry 50ml receiving flask centrally below the jet with the top of the neck a few
mm from the bottom of the jet. Open the orifice by lifting the ball valve and note the time
taken for the collection of 50ml oil with the help of stop watch. Note down the time taken is
seconds for the oil to get filled in the flask up to the red mark also note down the water and oil
temperature repeat the procedure for various temperatures using the same oil and tabulate the
readings.
OBSERVATIONS:-
Type of oil used:
Calculation of Density:
S.NO Weight of the empty jar Weight of the Volume of the Net weight of Density  =
W1 g jar with fluid jar in cc fluid W/V g/cc
W2 g
W= W2- W1 g
__________________________________________________________________________________
S.No Temperature in 0C Density of oil Time taken Kinetic Absolute
(g/cc) in Sec. Viscosity in Viscosity in
Water Oil Stokes poise
SAMPLE CALCULATIONS:-
The values obtained are
Temperature of the oil =
Density () of the oil =
Time for filling the 50ml of the oil =
Then Kinematic Viscosity (υ) = At – B/t centistokes
Where A & B are viscometer contains

A = 0.26,
B= 171.5,
t = time in seconds for collection of 50 ml of oil in the flask
The Absolute Viscosity = kinematic viscosity X Density =
RESULT: The Absolute Viscosity = ___________________in centipoises
__________________________________________________________________________________
Experiment-8
DETERMINATION OF SURFACE TENSION
Aim: To determine the effect if soap and detergent on the surface tension of water using a
Stalagmometer
Apparatus:
1. Stalagmometer
2. Volumetric flask
3. Small rubber tubing
4. Screw type pinch cock
Chemicals:
1. Detergent solution
2. Soap solution
Principle:
The size of the drop falling off from the end of tube depends on the surface tension of the
liquid and the size of the capillary end, which provides the line of attachment for the drop. Thus when
a liquid is allowed to flow through a capillaty tube, a drop will increase in size to a certain point and
then fall off. The total surface tension supporting the drop is 2r where r is the radius of the outer
circumference of the dropping end of the capillary tube. It is along this line that liquid, glass and air
meet and the force acting along the circumference, hence W = 2r, where W is the weight of the drop
and 2r is the circumference of the external wall of the capillary tube. The surface tension of the liquid
can therefore be determined from the weight of a single drop and the external radius of the dropping
tube.
If we have two liquids such that
W1 = 2r1 and
W2 = 2r2
then W1/W2 = 1/2
Thus the drop weight method can be employed for comparing the surface tension of two
different liquids. However, it is easier to count the number of drops formed by equal volumes to two
liquids than finding the weight of a single drop. For two different liquids, the weights of equal
volumes are proportional to their densities. Let N1 and N2 be the number of drops of liquid produced
from the same volume V of the two liquids.
Volume of a single drop = V / N1
Weight of a single drop = (V / N1) d1 or 2r1 = (V / N1) d1
Similarly for liquid 2
2 r2 = (V / N2) d2
Where d1 and d2 are the densities of the respective liquids. Dividing these two equations we get
1 /  2 = (N2.d1) / (N1.d2)
__________________________________________________________________________________
Procedure:
 Take a clean and dry Stalagmometer
 Attach rubber tubing with a screw pinch cock to the upper end of the stalagmometer to control
the flow of the liquid and clamp it to a stand.
 Make marks above and below the bulb with a marker pen if it is not marked.
 With the help of the rubber tubing, suck distilled water into the stalagmometer till the level
rises above the upper mark.
 Now allow the liquid to flow through the capillary (control the flow rate using the crew pinch
cock) and count the number of drops formed (N1) till the liquid level reaches the mark below
the bulb.
 Dilute the given stock soap solution ( 1%) to appropriate dilutions as given below using a
burette and determine the number or drops for each of these concentrations. Tabulate the data.
 Repeat the above procedure for 0.5, 0.1 and 0.05 % of detergent solution also and tabulate it as
above.
SNo Volume of water Concentration Exp.1 Exp.2 Average Surface

+ Volume of of (N) tension
soap/detergent soap/detergent (dynes/cm)
solution (ml) solution
1 50 + 0 Pure water
2 25 + 25 0.5 %
3 45 + 5 0.1 %
4 47.5 + 2.5 0.05 %
Calculations: Surface tension of water at 25°C = 72 dynes / cm

r1 = Surface tension of the reference liquid (i.e., water)
r2 = Surface tension of the test liquid
r1 = N2.d1
r2 N1.d2
Result : The surface tension of the given liquid = ……….dynes / cm
Precautions:
 Number of drops per minute must be in between 15-20
 The lower end of stalagmometer should be free from grease hence wash the stalagmometer first with
benzene or NaOH and then with chromic acid.
 Stalagmometer should be kept in a vertical position.
__________________________________________________________________________________
Experiment-9
IDENTIFICATION OF FUNCTIONAL GROUPS PRESENT IN ORGANIC COMPOUNDS
S.No Experiment Observation Inference

I PRIMARY TESTS:
a) State Solid /
Liquid
b)Colour Colourless liquid Aldehydes, ketones may be present
Yellow coloured liquid Nitro compound may be present
Colourless solid Acids, amides, anilides, carbohydrates may
be present
Brown (or) dark coloured Phenols, aromatic amines may be present
solid (or) liquid
c)Odour Pleasant Nitro compounds may be present
Phenolic Phenols may be present
Acidic acidic compound may be present
Aniline like smell Aromatic amines may be present
Oil of bitter almond Nitrobenzene, benzaldhyde may be present
II IGNITION TEST Smoky Aromatic compound
Non-luminous Aliphatic compounds containing low
percentage of carbon
Charring Compounds such as carbohydrate & its
salts get charred on ignition.
III SOLUBILITY:
Solubility test: One drop of the liquid or small quantity of the solid is dissolved in the following:
Experiment Observation Inference
a)Ether Insoluble carbohydrate/amide/imide/anilide may be
present
b)Water Soluble, solution is neutral carbohydrate may be present
to litmus
Solution turns blue litmus acidic compound may be present
red
c)Saturated NaHCO3 Soluble with effervescence Carboxylic acid may be present
solution and regenerated on
acidification with dil.HCl
Slow effervescence Polyhydric Phenols may be present
Slow effervescence & Nitro phenols may be present
solution turns Yellow
d)Dilute NaOH No characteristic change ketones, amines, aromatic nitro compounds
solution (changes in may be present
the cold are observed Dissolves readily in the Aromatic acids, phenols may be present
& heated if cold & substance is
necessary) regenerated on adding
conc. HCl
__________________________________________________________________________________
Dissolves & solution turns Nitro phenols, phenolic aldehydes may be
Yellow colour is removed present
on adding HCl
Dissolves readily forming a Carbohydrates may be present
Yellow or brown solution
on boiling
Dissolves in cold & Polyhydric phenols may be present
solution turns Yellow,
Brown & finally dark on
shaking
Ammonia gas is evolved Amides may be present
on boiling
Oily drops are formed with Anilides or Toluidines may be present
aniline like odour on
boiling
e) Dil. Na2CO3 Soluble with effervescence carboxylic acid may be present
Soluble without Phenolic Group may be present
effervescence
f) Dil. HCl Soluble and regenerates on Basic compounds like amines may be
adding alkali(NaNO2) present
g) Action of Conc. Blackening with Carbohydrates or certain hydroxyl aliphatic
H2SO4: To a small effervescence with the acids like Tartaric acid may be present
amount of organic evolution of CO and (or)
compound in a dry CO2 & SO2
test tube add conc. Blackening without Polyhydric Phenols like Resorcinol may be
H2SO4 and note the effervescence present
change in the cold CO and CO2 evolved, no Oxalates (or) Oxalic acid may be present
and then warm Blackening
gently.
IV Test for Un-saturation
a) Action of De-colorization of bromine Un-saturated compound
bromine in CCl4: to
1ml of bromine in No de-colourisation Saturated compound
CCl4, add drop of the
liquid or small
quantity of the solid.
b)Bayer’s Test: Decolourisation of KMnO4 Unsaturated compound
Add one drop of the with Brown ppt.
liquid or small
amount of the solid
to 1 ml of dil. No decolourisation of Saturated compound
KMnO4 KMnO4
c) Br water: 1 ml of Decolourisation Unsaturated compound
Bromine water add a
__________________________________________________________________________________
drop of Liquid or No Decolurisation Saturated compound
small quantity of
solid.
S.No Ether H2O NaHCO3 NaOH HCl H2SO4 Compound
1 + - + + - + Carboxylic acid
2 + - - - + + Base
3 + - - - - - Hydrocarbon
4 - + + + + + Carbohydrate
5 + - - - - + Neutral Compound
FUNCTIONAL GROUP ANALYSIS

A simple organic compound has one functional group but it may contain two or more
functional groups. All these commonly found functional groups have been divided into four groups.
The groups correspond to various elements in the organic compounds and are given below.
Type Elements present in compound Organic compound and its functional group
organic
1. a)C&H Hydrocarbons
b) C,H& O Carboxylic acid, phenol and alcohol(-OH),aldehyde,
ketone, ether and ester
2. a)C,H&N Amines
b)C,H,N& O Amides, nitro compounds & anilides
3. a)Halogens C,H,& X Halogenated hydrocarbons
b) Halogens and C,O,AX,O Acid halides,chloral hydrate.
4. C,H,S,O Sulphonic acid
ELEMENTAL ANALYSIS
C,H and O are considered as basic elements of organic compounds. Other than these three
elements, the elements that are most commonly present in organic compounds are nitrogen, sulphur
and halogens. The presence of these elements is detected by Lassaigne”s test.
Preparation of sodium fusion extract:

Heating procedure for liquids: Gently heat a small piece of freshly cut and dried sodium in an
ignition tube in the beginning and then to red hot. Remove the red hot ignition tube from the flame and
add one drop of the liquid. Repeat the heating process again until the tube becomes red hot, remove
and add another drop of the liquid. Repeat the operation two or three times.
Heating procedure for solids:

Gently heat a small piece of freshly cut and dried sodium in an ignition tube in the beginning
and then to red hot. Remove the red hot ignition tube from the flame and add a few milligrams of
solid. Repeat the heating process again until the tube becomes red hot. In the case of solids there is no
need to add the compound again.
Take 3 to 4 ml of distilled water in a mortar and immerse the red hot ignition tube into water.
Grind the ignition tube to pieces with the pestle, filter. Divide the filtrate into three parts and perform
the following experiments.
__________________________________________________________________________________
Compounds containing:
C,H,N,O,S, Halogen (X) + Na NaCN + NaOH + Na2S = NaX
Lassaigne”s Test:Test for Nitrogen: To one portion of sodium Bluish / Green Nitrogen
fusion extract add 2 drops of freshly prepared FeSO4 solution. Precipitate / colour present
Boil, cool and acidify with dil.H2SO4 with shaking until the Prussian blue colour Nitrogen
solution is clear. Now add few drops of FeCl3 No colour change absent
1) TESTS FOR CARBOXYLIC GROUP (-COOH):
S.NO EXPERIMENT OBSERVATION INFERENCE

1. Add 1 ml of saturated sodium CO2 gas evolved Carboxylic acid may
bicarbonate solution to 1 drop of the be present.
liquid or small amount of the solid No CO2 is evolved Carboxylic acid
absent.
2. Dissolve one drop of liquid or small Blue litmus changes Carboxylic acid may
amount of solid in 1 ml aqueous alcohol to red. be present.
and moisten the blue litmus paper
No colour change. Carboxylic acid absent
3. Esterfication: Dissolve one drop of Fruity odour Carboxylic acid
liquid or small amount of solid in 5 ml presence is conformed
of methyl/ethyl alcohol and add 2-3
drops of conc. H2SO4 and warm on
water bath and pour the content into
NaHCO3/Na2CO3 sol.
4. Phenolphthalein Test: Dissolve small Pink colour is Carboxylic acid
amount of the compound in water / obtained presence is conformed
alcohol. add a drop of phenolphthalein
and well diluted NaOH sol. drop wise
2) TETS FOR AMINES (-NH2):

1. Carbylamine test: add few drops of A foul smell of isocyanide is Amine may be
chloroform to about small amount of observed, by adding conc. present
the compound and add 2-3 ml of HCl smell can be destroyed.
ethanolic NaOH / KOH mix well and
warm gently.
2. Nitrous acid test: take small amount A brisk effervescence is Amine
of the given compound is 2 ml of dil. appeared. presence is
HCl and cool. Now add 10% aqueous conformed.
NaNO2 sol.
3. Diazotization test: dissolve small An orange red or a red dye is Amine
amount of the organic compound in 2-3 appeared. presence is
ml dil HCl cool under tap-water now conformed.
add 2 ml of 2.5 % NaNO2 solution, cool
again and add 1ml of alkaline β-napthol
sol.
__________________________________________________________________________________
3) TEST FOR HYDROCARBONS(C&H):

1. Sublimation test: To small amount Red colour is appeared Mono cyclic
of the compound add 3ml of hydrocarbon is
chloroform and shake well. Then conformed.
transfer a pinch of AlCl3 into a dry
test tube and sublime them by Blue or violet colour is Bicyclic hydrocarbon
adding above solution to the appeared. is conformed.
sublimed AlCl3 such that the
chloroform layer touches the AlCl3.
Green colour is appeared. Poly hydrocarbon is
conformed.
4) TEST FOR CARBOHYDRATES:

1. Blackening with H2SO4: heat small Immediately charring and Carbohydrate
amount of the compound in 1ml of blackening of the solution may be present
conc. H2SO4 . is observed.
2. 2, 4 DNP test: To small amount of Orange ppt. appears Carbohydrate

compound add 1 ml of water and add 1 may be present
ml of 2, 4 DNP reagents.
3. Molisch test: dissolve small amount of A deep violet coloured is Carbohydrate is

compound in 4 ml of water add 3-4 formed at the junction of conformed.
drops of alcoholic /-napthol and add two layers.
2 ml of conc. H2SO4 carefully from the
sides of the test tube.
__________________________________________________________________________________
5) TEST FOR CARBONYL COMPOUNDS:

1. 2,4-DNP test: An orange ppt of 2, 4- Carbonyl
To 2-3 drops of compound add 1 ml of the Dinitro phenyl compound is
2, 4-DNP reagent. Keep it in hot water bath hydrazone is formed. present
for few minutes.
2. Schiff’s test: No purple colour is Aldehyde group

To 1 ml of the compound add 5 ml of the developed is absent
schiffs reagent and heat the mixture on a
water bath for 2 minutes.
3. Tollen’s test: No silver mirror is Aldehyde group

To 1 ml of the compound add 5 ml of the deposited or no grey is absent.
tollens reagent and heat the mixture on a colour
water bath for 5 minutes.
4. Fehlings test: No red colour ppt is Aldehyde group

To 1 ml of the compound add 1 ml of formed. is absent.
Na2CO3 solution and 1 ml of the Fehlings
solution A and 1 ml of Fehling solution B.
Boil the mixture for 2-3 minutes.
5. Bisulphate test: White NaHSO3 product Ketone is

To 1 ml of the compound add 1 ml of is formed. present.
saturated Sodium bisulphate solution.
__________________________________________________________________________________
Experiment-10
PREPARATION OF ACETYL SALICYLIC ACID (ASPIRIN)
Aim : Preparation of Acetyl Salicylic Acid (Aspirin) with using salicylic acid.
Apparatus: 250 ml Round bottom Flask,

200 ml beaker,
Glass rod,
Funnel,
Dropper,
Filter papers,
Simple balance with weights
Chemicals Required: Salicylic acid,

Acetic Anhydride
Acetic acid
Conc. Sulphuric Acid (H2SO4) &
Distilled-water.
Chemical Reaction:
Procedure:
2.5 gms Salicylic acid and 5 ml Acetic anhydride taken in 200 ml Round Bottom Flask, mix
well, and add 1 or 2 ml Concentrated sulphuric acid . Heat it 50-600C on water bath for 10 to 15
minutes. Cool and add 100 ml water and filter the precipitate.
Result:
Yield =
Melting Point =
__________________________________________________________________________________
Experiment-11
DETERMINE THE RATE CONSTANT OF
HYDROLYSIS OF METHYL ACETATE
Aim: To determine the order of reaction and rate constant for the acid catalyzed hydrolysis of methyl
acetate.
chemicals: Methyl acetate,

0.5N HCL,
0.1NSodiumhydroxide,
Phenolphthalein indicator & ice.
Apparatus: Iodination flask 250ml,

Burette,
pippete10ml,
250 ml conical flask.
Principle:
Hydrolysis of methyl acetate is catalyzed by HCl. The rate of reaction is followed by titrating the
acetic acid formation during hydrolysis by sodium hydroxide at certain intervals of time.
Procedure:
 Fill the burette with 0.1N sodium hydroxide solution and fix to the stand. Take 90ml of 1NHCl
into an iodination flask and add 10ml of methyl acetate.
 Mix thoroughly for 5 to 10 seconds and note time.
 Immediately pipette out 10ml of the reaction mixture into a clean conical flask containing ice
and phenolphthalein indicator. Titrate it against 0.1N sodium hydroxide.
 Note the volume of sodium hydroxide required for titration as Vo pour the contents out, clean
the conical flask and keep it ready for next titration by adding cold water and indicator.
 After 10 mins of time pipette out another 10ml of the reaction mixture into the conical flask
and titrate against sodium hydroxide as before.
 Note the volume as V10.
 repeat the titrations at every 10mins of intervals upto 60 mins as V20,V30,V40 ,V50 and V60.heat
the reaction mixture on a water bath at 600c for 30 minutes cool and pipette out 10ml of
reaction mixture into a conical flask, add phenolphthalein indicator and titrate with sodium
hydroxide and note the volume as V
Graph: Plot a graph between Time (t) Vs Log (V-Vt ), Time (t) taken on X-Axis and Log (V-Vt )
taken on Y-Axis. Find out the slope, using slope to calculating K.
Result: the hydrolysis of acetic acid is a pseudo first order reaction the experimental value of K =
__________________________________________________________________________________
S.NO TIME Vol of NaOH V-Vt Log Log V-V0 K1 = 2.303/t Log V-V0
V-Vt ____V-Vt _______________V-Vt
Intial Final
__________________________________________________________________________________
Through Graph: Slope = S = y2-y1 =

x2-x1
K = 2.303 X S =
Activation Energy:
From the value of the reaction rate constant at two temperatures calculate the energy of
activation for the reaction using the equation:
Log K2 = -- E [ 1/T2 – 1/T1]

K1 2.303R
E= T1 T 2 X 4.567 X Log K2
T2 - T 1 K1
Result: The rate constant of the reaction (k) = ________.
The energy of activation (E) =_____________
__________________________________________________________________________________
Experiment-12
ADSORPTION OF CHARCOAL
AIM: To determine the Adsorption of aqueous acetic acid by Activated Charcoal and to study
adsorption isotherm.
APPARATUS: Stopper bottles,

20 ML Pipette,
Burette,
Beakers
CHEMICALS: Powdered activated charcoal,

0.5N Glacial acetic acid and 0.1 N NaOH.
PRINCIPLE: Freundlich adsorption isotherm is given by the expression:
x = KC 1/n - equation-1
m
Where ‘X’ and m are the amounts of solute (adsorbate) and adsorbent respectively, ‘C’ is the
equilibrium concentration of adsorbate. ‘K’ is a constant depends on both, the nature of adsorbent as
well as of adsorbate. “n” is another constant and depends only on the nature of adsorbate.
Taking log, the equation (1) can be written as
log x = log k + 1 log C

m n
When log X is plotted against log C, it gives a straight line whose slope is 1 and the
m n
Intercept log k.
PROCEDURE:
Proceed stepwise as follow:
1. Take 50, 40, 30, 20 and 10 ml of 0.5 N acetic acid in stopped bottles and to these add 0, 10, 20,
30 and 40 ml of distilled water respectively and label them.
2. Transfer 1 gm of activated charcoal to each bottle then shake these vigorously for about one
hour and allow them to stand for half an hour to attain the room temperature.
3. Filter off charcoal and while filtering discard initial nearly four ml filtrate in each case.
4. Take 5 ml of each filtrate and titrate it against standard solution of 0.1 N NaOH using
phenolphthalein as an indicator.
5. Note the reading in each case.
OBSERVATIONS:
1 .room temperature =. . . . . . °C
2. Amount of charcoal used in bottle = 1g
3. Volume of solution taken for titration each time = 5 ml
__________________________________________________________________________________
Bottle Volume of 0.5 N Volume of Initial Volume of
No CH3COOH (ml) water added normality of the NaOH used, V
acid (normality)
C2
1 50 0 0.50
2 40 10 0.40
3 30 20 0.30
4 20 30 0.20
5 10 40 0.10
Calculate the normality of the acid after adsorption using N1V1 = N2V2. Subtract this value from
initial normality of the acid. This will give you the normality of the acid adsorbed. Let it be N.
The amount of the acid adsorbed, x = N X 60 gm

1000
m = 1g in all cases
Repeat the calculation of remaining solutions and produce your results in tabular form as below:
Bottle Initial Normality of Amount of x/m log x / m log C

number normality acid adsorbed acid adsorbed
acid x
1 0.50
2 0.40
3 0.30
4 0.20
5 0.10
Plot the graph between x/m and log C. The slope is equivalent to 1 / n and the intercept to log k.
RESULT: The trend of the graph is in accordance with Freundlich adsorption isotherm. The values of
1 and ‘k’ are respectively……. and……. n
PRECAUTIONS:
1. Shake all the solutions properly and uniformly
2. Filter the solution before proceeding for titration and discard the initial small volume of the
filtrate.
3. Do not use wet filter paper in filtration as it may dilute the solution.
__________________________________________________________________________________

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Eng - Chemsitry Labmanual

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Engineering Chemistry Lab Manual (I B.

Tech Common to All)

Apparatus: 100 ml standard flask,

Chemicals Required: Ethylene di-amine tetra acetic acid (EDTA),

EDTA + Metal indicator complex  Metal ion-EDTA + Indicator

Preparation of standard hard water:

Standardization of EDTA solution:

Titration of Unknown Hard water:

Titration of Permanent hardness:

Preparation of Standard hard water solution:

W1 = Weight of bottle + substance = ____________ gms

W2 = Weight of bottle = ____________ gms

Weight of substance = (W1-W2) = ____________ gms.

Titration of Standard hard water

S.No Volume of Standard Hard Burette Reading Volume of EDTA solution

(20 ml Standard hard-water reacting with 20 ml 0.01M EDTA solution)

Titration of Sample Hard water:

Total hardness of water = 1000XV2

Titration of Permanent hardwater

Permanent hardness = 1000 X V3

Temporary hardness = 1000 X [(V2-V3)] =

Apparatus: 100 ml standard flask,

Chemicals Required: Brass sample,

2S2O3 + I2  S4O6- + 2I-

1. Preparation of standard potassium dichromate:

2. Standardization of sodium thiosulphate:

4. Weight of Brass Sample (B):

W1 = Weight of bottle + Brass sample = ____________ gms

W2 = Weight of bottle = ____________ gms

Weight of Brass Sample = B = (W1-W2) = ____________ gms.

Weight of the Brass Sample = B =

5. Preparation of Standard (K2Cr2O7)solution:

W1 = Weight of bottle + substance = ____________ gms

W2 = Weight of bottle = ____________ gms

Weight of substance = (W1-W2) = ____________ gms.

Normality of the solution = (W1-W2) X 10__ = (W1-W2) X 10 =

Standardization of sodium thiosulphate:

S.No Volume of standard Burette Reading Volume of

N1 = Normality of Potassium dichromate =

V1 = volume of Potassium dichromate = 20 ml

S.No Volume of Copper Burette Reading Volume of

N3= Normality of Copper solution = ?

V3 = volume of Copper Solution = 20 ml

Normality of Copper solution = N3= N4V4

1ml of 1N Na2S2O3 = 0.06354 g of Cu.

Percentage of Cu in the brass sample : (% of Cu in brass) = Z X 100 =

Apparatus: 100 ml standard flask,

Chemicals Required: Pyrolusite,

MnO2 + H2SO4 + H2C2O4  2CO2 + 2H2O + MnSO4

1ml of 1N KMnO4 = 1 ml of 1N Na2C2O4 = 0.04346 gm of MnO2 = 0.01099 gm of Mn

1 ml of 1N KMnO4 = 1 ml of 1N As2O3 = 0.04346 gm of MnO2

Preparation of Standard Di-Sodium Oxalate solution:

Standardization of KMnO4 solution:

W1 = Weight of bottle + substance = ____________ gms

W2 = Weight of bottle = ____________ gms

Weight of substance = (W1-W2) = ____________ gms.

Normality of the solution = (W1-W2) X 10 = __________X 10

Standardization of KMnO4 solution:

N1 = Normality of di sodium oxalate =

V1 = volume of di sodium oxalate = 20 ml

W1 = Weight of bottle + Pyrolusite = ____________ gms

W2 = Weight of bottle = ____________ gms

Weight of sample = (W1-W2) = __ gms. = _ mg