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MGM’S
Jawaharlal
PRINCIPAL Nehru Engineering
HOD College,
LAB INCHARG
LAB MANUAL
FIRST YEAR (EC & ES)
PRINCIPAL, HOD
Dr. S. D. Deshmukh Dr. V. M. Arole
2013
Lab Manual
To determine the relative viscosity of different liquid with respective water at different
9
temperatures.
Apparatus: - Beaker, Conical flask, glass rod, measuring cylinder, fractional weight box etc.
Chemicals: - Glacial acetic acid, 40 % formaldehyde solution, phenol, conc. HCl, Dist.water etc.
Theory: - Phenol resins are condensation polymerization product of phenolic derivative with
aldehyde (like formaldehyde, furfural) It is prepared by condensing phenol with formaldehyde in
presence of acid or alkaline catalyst.
Reaction:-
Step I:- Formation of ortho and para hydroxy benzyl alcohols from phenol and formaldehyde:-
OH OH
H2
OH C
O OH OH
C
H H H
H2C OH
Hydroxry,Benzyl Alcohols
OH OH
OH OH
H2 H2
H2
C OH C
C OH Heat/ -H2O
n
Novalac
Ortho-Hydroxy Benzyl Alcohol
n
Step III:- Formation of Bakelite from Novalac:-
OH OH
H2 OH OH
C H2
C *
H H Hexamethylene Tetraamine
H H
C O C O CH2 CH2
H H
H H
H2 H2
C C *
OH OH OH OH
Bakelite
Novalac
Procedure:-
1) Place 5 ml of glacial acetic acid and 2.5 ml of formaldehyde solution in 500 ml beaker.
Question-
6. Uses of Bakelite.
Experiment No: - 02
Aim: - To determine the acid value of given plastic material.
Chemicals: - Ethyl alcohol, Std. KOH solution, Plastic, Phenolphthalein, Acetone, Benzene etc.
Theory: - The acid value is number of milligrams of KOH which are needed to neutralize the acidity
present in 1 gr of material. For its determination material is dissolved on suitable solvent usually
neutral ethyl alcohol. It is then titrated against standard alkali solution (0.1 N KOH) using
phenolphthalein as an indicator. Acid value is calculated by formula,
Procedure:-
1) Weight exactly around 5 gr of the sample on watch glass and dissolved it into 50 ml of neutral
ethanol.
2) Heat the solution for one minute in water bath then cool it.
4) Titrate the solution with 0.1 N KOH till the color of solution is faint pink color.
Observation Table:-
Sr. No Weight of Sample (in gm) Burette reading (in ml) Mean
Questions-
3. What happen? When acid value of sample is more than permissible value.
Experiment No: - 03
Aim: - To determine neutralization number of Oil.
Chemicals: - Ethyl alcohol, Std. KOH solution, Oil, Phenolphthalein, Acetone, Benzene etc.
Theory: - The acid value of lubricating oil is defined as number of milligrams of KOH required to
neutralize the free acid present in one gram of oil sample. In good lubricating oil acid value should
minimum increase in acid value should be taken as an indicator of oxidation of oil which may lead to
gum and sludge formation decides corrosion. A known weight of oil sample is dissolved in a suitable
solvent and titrates with a standard alcoholic KOH solution.
Reaction:-
Procedure:-
In to 50 ml of neutral ethanol.
2) Heat the solution for 30 minute in water bath cool it and add 2 to 3 drops of
Phenolphthalein indicator.
3) Titrate the solution with 0.1 N KOH till the color of solution is faint pink color.
Observation Table:-
Formula:-
Calculations:-
Question:-
1. Explain the properties of good lubricant.
3. What happen? When acid value of lubricant is more than permissible value.
4. Why the acid value of lubricant is determined before using in lubrication process?
Experiment No: - 04
Aim: - To find the normality of hydrochloric acid and acetic acid by titrating the mix of HCl &
CH3COOH against sodium hydroxide solution conductometrically.
Chemicals: - Hydrochloric acid, Acetic acid, Sodium hydroxide, distilled water etc.
Theory: - Conductometry can be used to determine the end point of a titration. This method is based
on the measurement of conductance during the course of titration. The conductance varies
differently before and after the equivalence point. This is due to the reason that electrical
conductance of a solution depends upon the number of ions present and their ionic mobility’s i.e.
speeds. When conductance values plotted against volume of titrants added, U shape is obtain, the
point of intersection of lines gives the end point.
Reaction:-
Procedure:-
1. Prepare the 10 ml mixture of 5ml hydrochloric acid solution and 5ml of acetic acid solution in a
beaker. Add few ml of distilled water in it.
2. Immerse the conductivity cell in the solution so that the electrodes completely dip in solution.
4. From the burette add 0.3N NaOH solution in 0.5 ml lots with continuous stirring and measure
the conductance of solution at each 0.5ml addition of NaOH.
5. Plot a graph between observed conductance values along y-axis against the volume of alkali
added along x-axis. The end point of intersection gives the amount of alkali required for
neutralization of acid.
Observation Table:-
Sr.No. Volume of NaOH added (in ml) Observed conductance (in mhos)
1 0 ml
2 0.5 ml
3 1 ml
19 9 ml
20 9.5 ml
Calculations: -
N1 × 5 = 0.3 × V2 N3 × 5 = 0.3 × V4
Result: -
Question -
1. What is mean by conductance?
5. After neutralization of both acids excess of NaOH added what is the effect on conductance
Experiment No: - 05
Aim: - Determination of cell constant of a conductivity cell.
Theory: - Conductance is the reciprocal of resistance. It is depend upon three factors, number of ions,
and nature of ions and mobility of ions towards their respective electrodes. The specific conductance
of electrolyte is decreased by increasing its dilution and equivalent conductance is increased by
increasing its dilution. The observed conductivity of an electrolyte will be equal to its specific
conductivity if cell constant is one.
Procedure: - Connect conductivity cell to Conductivity Bridge and keep the cell deepen in distilled
water.
Prepare the solutions of 0.1, 0.01, 0.02, 0.005 and 0.001 N of KCl.
Note down the conductance of 0.1 N and 0.02 N KCl solutions by using conductometer and
determine the cell constant.
PART II –
Determine the conductance of all prepared KCl solutions and calculate the specific and equivalent
conductance of each solution.
Formula:-
Specific conductance
K × 1000
Equivalent Conductance = C
Observation Table:-
PART I –
PART II –
Calculations:-
1) Specific conductance:-
2) Equivalent Conductance:-
Result: - The cell constant of the given conductivity cell is = ………………… /cm
Question-
1. Define the term Specific & equivalent conductance?
Theory: - In hard water sample the total hardness can be determined by titrating the Ca2+ and Mg2+
present in an aliquot of the water sample at pH10 with EDTA using EBT indicator. Permanent
hardness can be determined by precipitating the temporary hardness by prolonged boiling followed
by titration with EDTA solution. The difference in the titre values corresponds to the temporary
hardness of the water sample.
When Eriochrome Black-T dye is added to the hard water at pH around 10 it gives wine red colored
unstable complex with Ca2+ and Mg2+ ions of the sample water. Now when this wine red-colored
complex is titrated against EDTA solution (of known strength) the color of the complex changes from
wine red to original blue color showing the end point.
Reaction:-
O O
H2 H2
HO C C H2 H2 C C OH
N C C N
HO C C H2C C OH
H2
O O
EDTA
Ethylene diamine tetra-acetic acid
Ca2+ Ca2+
Mg2+ Mg2+
Ca2+ Ca2+
Mg2+ Mg2+
2. Add 5 ml of buffer solution and 2 to 3 drops of EBT indicator, the color of solution turns wine
red. Titrate the flask solution against standard EDTA solution from the burette until the color changes
from wine red to blue at the end point. Take at least two concordant readings. Let the volume of
EDTA solution used = V1 ml
3. Titrate similarly unknown hard water and find out volume of EDTA solution used. Let the volume
of EDTA used with unknown hard water = V2 ml
4. Take 250 ml of the hard water sample in 500 ml beaker & boil gently for about one hour, cool,
filter into a 250 ml measuring flask & make the volume up to the mark with distilled water. Take 25
ml of this solution and proceed in the same way as in step (2). The volume of EDTA used (V3)
corresponds to permanent hardness of the water sample. Temporary hardness is calculated by
subtracting permanent hardness from total hardness. Let volume used = V3 ml
Observation Table:-
1 10 ml
2 10 ml
3 10 ml
1 10 ml
2 10 ml
3 10 ml
3. For Boiled Water: -
1 10 ml
2 10 ml
3 10 ml
Calculations:-
=V1 × 100×0.01
=V2 × 100×0.01
Mg (HCO3)2 Boil ?
Experiment No: - 07
Theory: - The pH value of solution is defined as negative logarithm of hydrogen ion concentration. It is
expressed in gram/ion lit.
Consequently, PH of neutral solution is 7; in acidic solution PH<7, since [H+]>10-7 on the other hand PH
of the alkaline sol.n is >7, Since [H+] <10-7
pH of the sol.n is tasted by using pH paper. This gives different colour with different values.
Procedure:
2) Deep the pH electrode in the Beaker & note down the pH.
3) Then take the another solution in a beaker deep the electrode & note pH of solution also
deep the pH paper & observe the colour Change& note down the nature of solution.
4) Take the four different reading of four different solutions & Write the result either the solution
Result: - 1) pH of first unknown solution is ------ hence the nature of solution is --------
Question:-
This corrosion occurs due to existence of separate anodic and catholic part between which current
flows to the conducting solution. When there is acidic environment evolution of hydrogen gas takes
place. Thus this type of corrosion causes displacement of hydrogen ions from all acidic solution by
metal ions.
All metals above hydrogen in electrochemical cells have a tendency to get dissolved in acidic
solution with simultaneous evolution of hydrogen gas.
Daniel cell consist of Zinc electrode dipped in Zinc Sulphate solution (Oxidation takes place) and
Copper electrode dipped in Copper Sulphate solution (Where reduction takes place).
Zn / ZnSO 4 // CuSO4 / Cu
Zinc is present at higher stage in electrochemical series hence oxidation occurred at Zinc
electrode and Zinc get corrode.
Diagram:-
Galvanic Cell
Conclusion:-
Question-
Theory: - The property of resistance to flow when a stress is applied to a liquid is called “Viscosity”. In the
process of flow the molecule comprising the fluid move fast one another and viscosity arises from what can
the termed the frictional effect of relative motion. When the liquid is flowing to a circular tube the flow
pattern is called streamlines or viscous or laminar. The viscosity is increased by increasing molecular weight
and decrease by increasing the temperature.
Formula: - n = ℓ2 / ℓ 1 × t2/t1 × n1
Procedure:-
1) Clean the viscometer with chromic acid and then wash thoroughly with distilled water. It & finally washed
with acetone and dried.
2) A sufficient volume of distilled water is introduced by pipette in bulb B so that the bent Portion of tube
and half or a little more than a half of bulb B is filled up.
4) Trough the rubber tube attach to upper arm of bulb A, suck up water until it rises above the upper mark
C and allow it to flow under its own weight.
5) The time of flow of water from C to D is continued by starting the stop watch as the Meniscus just
reaches upper mark C and stopping the watch as the meniscus just passes the lower mark D.
6) Take at least three reading of water at different temperature. Also take the similar reading of ethanol at
various temperatures.
Observation Table:-
Result: - The relative viscosity of the liquid with respective with water at 250C temperature
Question:-
1. Define term viscosity.
Chemicals: - Formaldehyde (40%), Urea, Conc. Sulphuric acid, dist. Water etc.
Theory: - Urea resins are condensation polymerization product of urea with formaldehyde. It is
prepared by condensing urea with formaldehyde in presence of acid or alkaline catalyst.
Reaction:-
O
C H H2
H H2
i) O O N C OH H H N C OH
Heat
C C O C O C H2
NH2 HN C OH
H2N NH2 H H
H2 H2
N C N C N
O O Heat O C
n O C O C
n C H2 H2
iii) C C N
H2N NH2 N C N
H H
Formaldehyde Urea
Urea Formaldehyde
Procedure:-
2) Add about 2.5gr of urea while stirring until a saturated solution is obtain.
3) Add a few drops of concentrated sulphuric acid with stirring continuously during addition.
5) When the reaction is complete wash the residue with water and dry the product and calculate the
yield of the product formed.
Chemicals:- Conc. HCl, Sodium hydroxide, potassium iodide, MnSO4, Sodium Azide, 0.1 N Sodium
thiosulphate , water sample.
Theory: - Oxygen dissolved in water to the extent of 7-9 mgs/lit at a temperature range of 250 -350 C.
The estimation of dissolved oxygen in water is useful in studying corrosion effect of boiler feed water
and in studying water pollution. The amount of dissolved oxygen in water is estimated using winkler’s
reagent (potassium bromide + Potassium bromated).
Water sample is collected carefully aeration/deaeration in ground stopperd flask. Initially manganese
sulphate and alkaline-iodide reagents are added and the reaction occur as follows
2KOH + MnSO4 → Mn (OH)2 + K2SO4
Procedure:-
1. Take 50 ml water sample in a iodine flask.
2. Add to it 1ml of MnSO4solution and 1ml of basic KI solution.
3. Shake it, the precipitate is allowed to settle down half a way and shake again. Repeat the
procedure for three times.
4. Then add 1ml of Conc. H2SO4 to dissolve the precipitate.
5. Then add 2-3 drops of starch indicator.
6. Titrate the solution against the thiosulphate solution till colour changes from blue to colourless.
Observations:-
In conical flask: - 50ml water + 1ml of MnSO4 solution + 1ml of basic KI solution
In burette: - 0.1 N Sodium thiosulphate
Indicator: - Starch
End Point: - Blue to Colorless
Observation table:-
1. 50 ml
2. 50 ml
3. 50 ml
Calculations:-
V1N1=V2N2
N2= V1N1/V2
=……………ml × ………..N/50
= ………………..mgs/lit
Question:-
1 What is the role of buffer solution?