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GREATER NOIDA
LIST OF EXPERIMENTS
SUBJECT CODE
AS103/AS203: ENGINEERING CHEMISTRY (THEORY)
AS103P/AS-203P: ENGINEERING CHEMISTRY (PARACTICALS)
To Write in Practical File
Left Hand Side with Pencil
Date
Aim:
Observation Table:
S.No Volume in the
Burette Reading(ml)
Titration Flask(ml)
Initial
Final
1
2
3
(This table is only for volumetric titrations)
Graph if required:
Calculations:
Result:
EXPERIMENT No -1
OBJECT: Introduction to safety and working in a chemical laboratory
APPARATUS: First Aid Box
PROCEDURE: All too often chemical laboratories are the scene of accidents, mostly minor ones
but some of serious nature. These are caused by the carelessness of the experimenter, defects of
equipment and improper procedures.
Preventive Measures or Habits of Safety
The following precautions, if they are observed sincerely, would avert the most mishaps
1.
Come to laboratory well prepared. For this, read the theory, procedure and
precaution of the experiment to be performed.
2.
Never work alone in the laboratory. A minor mishap may be serious if you are alone.
3.
Never touch or taste any chemical as most of chemicals are poisonous and corrosive
to skin. Use spatula or paper spoon for solid and dropper or glass tube/rod for liquid
chemicals.
4.
Keep the mouth of the test-tube away from you as well as from your neighbor while
heating the liquid contained in it.
5.
6.
Strong oxidizing agents and easily oxidized materials must be mixed with extreme
caution and in small amounts. The reaction between HNO3 and organic reducing
can be so violent that a dangerous explosion may result.
7.
3. Eye Injuries
(i)By a solid
4. Fires
(a)
5. Inhalation of poisonous fumes and Remove the victim to the open air and loosen
clothing at the neck. If breathing has stopped,
gases
give artificial respiration until help arrives.
EXPERIMENT NO:- 2
OBJECT: Determination of hardness of water by titration with standard EDTA solution
APPARATUS: Burette, Pipette, Conical Flask, Beaker Measuring cylinder.
CHEMICALS: N/100 EDTA Solution, Water sample, Eriochrome Black-T
Buffer Sol. (pH = 10)
THEORY: When Eriochrome black T (indicator) is added to hard water solution at around pH 10,
it forms wine red colored unstable complex with Ca2+ and Mg2+ ions of the sample water. When
this wine red colour solution is titrated against EDTA solution, the colour of the solution changes
from wine red to blue colour at the end point.
Ethylene diamine tetraactic acid (EDTA) is a well knowing complexing agent which is widely used
in analytical work, on account of its powerful complexing action and commercial availability.
PROCEDURE: Take 10 ml of hard water sample in a conical flask with help of a pipette. Add 5
ml of buffer solution. Add 5 drops of Eriochrome black-T indicator .Colour of the solution turns
wine red. Titrate the solution against EDTA until the colour changes from wine red to blue. Repeat
the titration for two concordant readings. This reading corresponds to total hardness.
Take about 250 ml of the hard water in 500 ml beaker and boil it for half an hour, cool it and titrate
the solution as mentioned above for permanent hardness. Repeat the titration for two concordant
readings
OBSERVATION:
Normality of EDTA solution = N/100
1.
Indicator used
End point:
Erichrome Black- T
Wine red Blue
OBSERVATION TABLE:
For Tap Water to estimate Total Hardness
S.No Volume of tap water in the
Titration Flask(ml)
1
2
3
Burette Reading(ml)
Initial
Final
Volume of N/100EDTA
Solution used from burette(ml)
Volume of N/100EDTA Solution used from burette (ml) to neutralize10 ml of water sample =v2ml
For Boiled Water to estimate Permanent Hardness
S.No Volume of boiled water in the
Titration Flask(ml)
1
2
3
Burette Reading(ml)
Initial
Final
Volume of N/100EDTA Solution used from burette (ml) to neutralize10 ml of boiled water =v3ml
CALCULATION:
a)
Calculation of Total Hardness :Equivalents of Ca+2 &Mg+2 in the water sample = Equivalents of EDTA consumed.
N1V1=N2V2
(water)
(EDTA)
N1= (1/100xv2ml)/10ml
Strength of total hardness causing ions in terms of CaCO3 ions = N1x50 gm/litre
= N1x50 x1000mgm/litre (in terms of calcium carbonate)
= N1x50x1000ppm
Calculation of Permanent Hardness :Equivalents of Ca+2 &Mg+2 in the water sample = Equivalents of EDTA consumed.
N1V1=N2V2
(water)
(EDTA)
N1= (1/100xv3ml)/10ml
b)
c)
RESULT:
Total Hardness
Permanent Hardness
Temporary hardness
S1
= ___________________ ppm
S2
= ___________________ ppm
S1 - S2 = ___________________ ppm
PRECAUTONS:
1.
2.
3.
4.
5.
EXPERIMENT NO:- 4
OBJECT: . Determination of Alkalinity in water sample.
APPARATUS: Beaker, Pipette, Burette, Conical Flask
CHEMICALS: Alkalinity Sample, 0.1N HCl, Methyl Orange and Phenolphthalein.
THEORY: The alkalinity in water is due to the presence of hydroxyl ion (OH-), carbonate ion
(CO32-) and bicarbonate ion (HCO3-) present in the given sample of water. These can be estimated
separately by titration against standard acid, using phenolphthalein and methyl orange indicators.
The chemical reaction involved can be shown by the equations given below:
i)
OH- + H+ H20
ii)
CO32- + H+ HCO3iii)
HCO3- + H+ H20 + CO2
PROCEDURE: Take 10ml of the sample solution in conical flask with help of a pipette. Add 2-3
drop of phenolphthalein indicator. Titrate this sample against HCl solution until the pink colour
caused by phenolphthalein just disappears. Note down this reading as phenolphthalein end point.
Now add 2-3 drops of methyl orange indicator in the same solution. Continue the titration until
yellow colur change into pinkish orange. Note the volume of acid used. This is methyl orange end
point.
OBSERVATION:
1.
2.
OBSERVATION TABLE:
For Phenolphthalein Indicator
S.No Volume of alkalinity sample
in the Titration Flask(ml)
1
2
3
Burette Reading(ml)
Initial
Final
Volume of N/10HCl Solution used from burette (ml) to neutralize10 ml of alkalinity sample =V1ml
For Methyl Orange Indicator
S.No Volume of alkalinity sample
in the Titration Flask(ml)
1
2
3
Burette Reading(ml)
Initial
Final
Volume of N/10HCl Solution used from burette (ml) to neutralize10 ml of alkalinity sample =V2ml
(This is total volume starting with pink colour to colourless and then yellow to pinkish orange)
CALCULATIONS:
Volume of water sample solution taken in titration flask = 10 ml.
Volume of HCl used for Phenolphthalein end point = V1ml
Volume of HCl used for methyl orange end point = V2ml
Equivalents of OH-+ equivalents of CO32- = Equivalent of HCl in V1 of N/10 HCl (1)
Equivalents of OH-+ equivalents of CO32- = Equivalent of HCl in V2 of N/10 HCl (2)
Solving equation (1) & (2)
2Equivalents of CO3 = 2(V2-V1) of N/10 HCl
Equivalents of OH- = (2V2-V1) of N/10 HCl
1) Calculation of alkalinity due to OHStrength of OH- = (2V2-V1)/(10x10) equivalent/L
Strength of OH- in terms of CaCO3 = (2V2-V1)/100 x50x1000 mg/l
=500(2V2-V1) ppm (in terms of CaCO3)
2) Calculation of alkalinity to Na2CO3
Strength of CO3- = 2(V2-V1)/10x10 equivalent/L
=2(V2-V1)/100 x50x1000 mg/l
=1000x (V2-V1) ppm (in terms of CaCO3)
RESULT:
ppm.
ppm.
ppm
PRECAUTONS:
1.
2.
3.
4.
5.
10
EXPERIMENT-5
OBJECT: Determine the rate constant of hydrolysis of an ester such as ethyl acetate catalyzed by
an acid.
APPARATUS: Thermostat, conical flasks with cork, burette, pipette, stop watch,
CHEMICALS: Ethyl acetate, 0.5 M HC1, 0.1 M NaOH, phenolphthalein indicator.
THEORY:
The hydrolysis of ethyl acetate gives ethyl alcohol and acetic acid
CH3COOC2 H5 + H2O CH3COOH + C2H5OH
The reaction is catalyzed by dil.Hyhrochloric acid and is a reaction of first order as the
conc. Of water is in large amount and does not change significantly during the reaction.It is
pseudomolecular reaction.
The rate constant is determined by using the following kinetic equation of first order
2.303
a
log
t
ax
11
PROCEDURE: (i) Take 100 ml 0.5 M HCl in a dry 250 ml conical flask cork and keep it on water
bath at room temperature, also take about half test tube of ethyl acetate in conical flask and place it
on the water bath at the same temperature of the water bath.
(ii) Rinse the burette and Fill a burette with 0.1 M NaOH solution, Take 3-4 conical flasks
containing about 250 ml of ice cold water or small pieces of clean ice.
(iii) pipette out 5 ml of the ester and add it to the flask containing 100 ml of 0.5N HCl
acid.
(iv)Shake well and pipette out 10 ml sample of the reaction mixture into a conical flask
containing ice cold water,titrate this against 0.1N NaOH using phenolphthalein indicator
appearance of pink colour is the end point. The volume of NaOH used against the sample at the
start of the reaction and is taken as V0.
(v) Note the time of draining out 10 ml of solution into the flask and if it is 10
sec.then
the mixture should be added to the ice water 5 minutes early than 10 mins.
(vi) pipette out 10 ml of the solution and add it to the flask containing chilled water after 10
mins.Titrate it against 0.1N NaOH this is Vt after 10 mins.
(vii)
Repeat the procedure after every 10 mins.for atleast four readings there should be an
increase of 5 mins for every reading i.e. at intervals of 10, 20, 30 and40 min.
(viii)
Finally remove the flask from water bathand place it on a water bath at 50-60oC for
about an hour.
pipette out 10 ml of the reaction mixture and titrate it against 0.1N NaOH this is V.
OBSERVATION:
Temperature of the water bath = ... C
S.No
Burette Readings
Time in min. Initial Reading FinalReading Vol. of NaOH
used
CALCULATION:
2.303
a
log
t
ax
12
RESULT:
The rate constant for acid catalyzed hydrolysis of ethyl acetate is ..min-1.
PRECAUTIONS:
(i) Temperature of reaction mixture should be constant throughout the course of the reaction.
(ii)
The reaction must be stopped before carrying out the titration of the sample by adding it to
13
Experiment-6
PROCEDURE:
(a ) Preparation of neutral formalin solutionIn a conical flask take 50 ml of 40% formalin
solution and add about 10 drops of phenolphthalein solution To it add very carefully from a burette,
a solution of dilute sodium hydroxide till the solution is just faintly pink.
(b)
Titration of the given glycine solution Take 10 ml. of the given glycine solution in a
from the burette drop by drop with continuous shaking, till the solution is just faintly pink. To this
neutralized solution add about 4ml. neutralized formalin solutionthe pink colour of the solution
disappears immediately and the solution becomes markedly acidic. Now note the initial reading of
the burette and titrate the acidic solution with sodium hydroxide solution till pink colour is just
restored.
(c)
Titration with standard glycine solutionRepeat the above procedure with the standard
glycine solution.
14
OBSERVATION:
(a) Titration with given glycine solution
S.No.
Burette reading
Initial
NaOH solution
Initial
used
1.
10.0 ml.
....ml.
2.
10.0 ml.
....ml.
3.
10.0 ml.
....ml.
(b)
S.No.
Burette reading
Initial
NaOH solution
Initial
used
1.
10.0 ml.
....ml.
2.
10.0 ml.
....ml.
3.
10.0 ml.
....ml.
CALCULATION:
(i)
Strength of the standard glycine solution =
(ii)
A gm/L
RESULT:
The strength of the given glycine solution = gm/L
PRECAUTIONS:
(i) During the neutralization of formalin and glycine solution, excessive addition of sodium
hydroxide solution should be avoided, as it is not accounted in the calculations.
15
Experiment- 7
OBJECT: Synthesis of benzimidazole and record of its UV spectrum.
CHEMICALS: 0-Phenylenediamine, Formic acid, Sodium hydroxide (10%)
THEORY: 0-Phenylenediamine condenses with formic acid to yield benzimidazole
PROCEDURE: Take 2 gm of 0-phenylenediamine in a round bottom flask and add 1.2 ml of 70%
formic acid. Heat the mixture on a water bath at 1000C for two hours. Cool and add 10% NaOH
solution with constant stirring until the mixture is just alkaline. Filter the product, wash with cold
water and dry at 1000C . Report the yield .
Yield:
gm
UV Spectrum of Benzimidazole.
16
EXPERIMENT- 9
AIM: To determine the neutralization number (acid value) of a given sample of oil.
CHEMICALS:
THEORY: The neutralization number or Acid value of lubricating oil idefined as the number of
milligrams of KOH required to neutralize the free acid in 1 gm of the oil sample.
Acid value should be less than 0.1 for lubricating oil. 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. A
known wt. of the oil sample is dissolved in a suitable solvent and titrated with a standard alcoholic
solution of KOH to definite end point.
H+ + OH- H2 O
(1)
(2)
PROCEDURE: Take 3 ml of oil sample in a titration flask and dissolve it in a minimum quantity of
alcohol. Now add 2-3 drops of phenolphthalein and titrate against KOH (N/100) solution taken in a
burette. The appearance of pink colour represents the end point .The experiment is repeated 3-4 times
with oil sample for getting concordant readings.
Same procedure is also repeated with the solvent alone as a blank titration.
OBSERVATION :
(i)
Initial Reading
(Burette)
Final Reading
(Burette)
Vol. of KOH
Used. (A)
Initial Reading
(Burette)
Final Reading
(Burette)
Vol. of KOH
Used. (B)
1.
2.
3.
17
CALCULATIONS:
Acid Value
RESULT:
(A-B) x 1/100 x 56
-------------------------3
18
EXPERIMENT N O:- 10
OBJECT: Detection of functional groups in an organic compound by wet tests
APPARATUS: Test tubes, beaker, Test tube holder
CHEMICALS: Distilled water, Samples with required functional groups
Sodium bicarbonate solution, Neutral Ferric chloride solution, Sulphuric Acid, Sodium Hydroxide,
Phthalic anhydride, Sodium Metal, Na2SO4, Ethanol, Sodium nitroprusside, etc.
Theory: Test for Functional Groups:SL.
Experiment
I
For Carboxylic Acid
2
Take a few drops sample and add 5 ml of cold
NaHCO3 solution. in water
3
To a part of original solution add 5 drops of
ethyl alcohol and conc. H2SO4 and lead
acetate
II
For Phenols
1
To a part of alcoholic solution of original
solution and 2-3 drops of aq. FeCl3 solution.
Observation
Effervescence due to
the evolution of CO2
A fruity smell of ethyl
ester
-COOH
Violet phenol
(O-cresol or Pcresol)
Blue Violet
(Resorcional)
Shows the
presence of
Phenol.
III
1
For Carbohydrate
2
3
IV
1
V
1
Inference
A red or crimson
colour
An immediate charring
A reddish violet ring at
the junction of the two
liquid is formed.
-COOH
presence of
carbohydrate
presence of
carbohydrate
presence of
carbohydrate
For Ketones
Take 2 ml of aqueous or alcoholic solution of
original solution, and add 0.5 ml of Sodium
nitroprusside and 2-3 drops of aq. NaOH
Take 1 ml alcoholic solution of original
solution and add 1 ml of 2;4-dinitro phenyl
hydrazine solution, boil and cool
presence of a
Ketone
presence of a
Ketone
A red precipitate of
Cu 2O is obtained
presence of
and aldehyde
For Aldehyde
Take 1 ml of a mixture of equal amounts of
Fehling solution A & B, and add a few drops
of original solution and heat on a water bath
19
for 5 minutes.
Take 1 ml of Tollens reagent and a few drops A silver mirror is
of original solution and heat on a water bath
obtained due to
for 5-10 minutes.
deposition of metallic
silver on the side of the
test tube.
presence of an
aldehyde.
RESULT:
1. Sample-1 contains-------------2. Sample-2 contains-------------3. Sample-3 contains-------------4. Sample-4 contains-------------5. Sample-5 contains--------------
PRECAUTIONS:
1. All the test tubes should be cleaned properly
2. All the reagents should be freshly prepared
3. Test tubes should be hold away from the face
20