ENGINEERING CHEMISTRY LAB MANUAL
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Engineering Chemistry Lab Manual
Page | 2 B V Raju Institute of Technology (UGC Autonomous)
Engineering Chemistry Lab Manual
Page | 3 B V Raju Institute of Technology (UGC Autonomous)
List of Experiments: Titrimetry: 1. Estimation of ferrous iron by dichrometry. 2. Estimation of hardness of water by EDTA method. Mineral analysis: 3. Determination of percentage of copper in brass. 4. Estimation of manganese dioxide in pyrolusite. Instrumental Methods: Colorimetry: 5. Determination of ferrous iron in cement by colorimetric method 6. Estimation of copper by colorimetric method. Conductometry: 7. Conduct metric titration of strong acid vs strong base. 8. Conduct metric titration of mixture of acids vs strong base. Potentiometry: 9. Titration of strong acdvs strong base by potentiometry. 10. Titration of weak acid vs strong base by potentiometry. Physical properties 11. Determination of viscosity of sample oil by redwood / Oswald’sViscometer 12. Determination of Surface tension of lubricants. Preparations 13. Preparation of Aspirin 14. Preparation of Thiokol rubber Adsorption: 15. Adsorption of acetic acid on charcoal. TEXT BOOKS: 1. Practical Engineering Chemistry by K. Mukkanti, etal, B.S. Publications, Hyderabad. 2. Inorganic quantitative analysis, Vogel. REFERENCE BOOKS: 1. Text Book of engineering chemistry by R. N. Goyal and HarrmendraGoel, Ane Books Private Ltd., 2. A text book on experiments and calculation Engg. S.S. Dara. 3. Instrumental methods of chemical analysis, Chatwal, Anand, Himalaya Publications
Engineering Chemistry Lab Manual
Page | 4 B V Raju Institute of Technology (UGC Autonomous)
GENERAL PRECAUTIONS TO BE TAKEN IN THE
LABARATORY
1. Never work in the laboratory unless a demonstrator or teaching assistant is present.
2. Do not throw waste such as match stems filter papers etc. into the sink. They must be
thrown into the waste jars.
3. Keep the water and gas taps closed expect when these utilities are needed.
4. Never taste any chemical unless instructed to do so and don’t allow chemicals to come
in contact with your skin.
5. While working with gases, conduct the experiment in a fume hood.
6. Keep all the doors and windows open while working in the laboratory.
7. You should know about the hazards and properties of every chemical which you are
going to use for the experiment. Many chemicals encountered in analysis are poisonous
and must be carefully handled.
8. Sulphuric acid must be diluted only when it is cold .This should be done by adding it
slowly to cold water with stirring ,and not vice versa.
9. Reagent bottles must never be allowed to accumulate on the work bench. They should
be placed back in the shelves as and when used.
10. Containers in which reaction to be performed a little later should be labeled. Working
space should be cleaned immediately.
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INSTRUCTIONS FOR RECORD WRITING
1. Write on the right hand page the following order:
a) Serial number and date of performance (in the margin)
b) Name and number of the experiment as given in the list.
c) Aim of the experiment.
d) Description of the apparatus.
e) Procedure including sources of error and precautions taken to eliminate or to
minimize them.
f) Inference or Result.
g) Explanation, if necessary of any divergence in the expected result.
2. Left hand page should contain the following in their proper places.
a) Neat diagram of the main apparatus.
b) Observation in tabular form.
c) Calculation in tabular form.
d) Graph sheets and other papers to be attached.
3. Students should submit a record of the previous experiments when they come for
practical work.
4. An experiment is deemed to be complete when it is satisfactorily performed and
recorded.
KEEP THE RECORD BOOK NEAT IT FETCHES MARKS.
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VOLUMETRIC ANALYSIS
BASIC CONCEPTS OF VOLUMETRIC ANALYSIS
Chemical analysis of the compounds is carried out in two ways
1. Qualitative analysis.
2. Quantitave analysis.
Qualitative analysis shows what element a given contains.
Quantities analysis determines the quantity of a particular component present in substance.
It is carried out in two ways
1. Gravimetric analysis.
2. Volumetric analysis.
Gravimetric analysis involves the estimation of the amount of a given compound from the
results of weighing.
Volumetric analysis is based on the measuring the volume of the solution of a substance.
Terms involved in volumetric analysis
1. Titration: The process of finding out the volume of one of the solution required to react
completely with a definite volume of one the other solution of known concentration is called
titration.
2. Titrant: The solution of known strength is called titrant.
3. Titrate: The solution whose concentration to be estimated.
4. Indicator: The reagent which indicates the endpoint or equivalent point of the titration.
The strength of concentration of a solution is expressed in the following ways.
NORMALITY:
Number of gram equivalents of the substance dissolved per liter of the solution is called
Normality.
It is denoted by N
Normality = Wsolute/Esolute × 1/Vsovent (in lit)
Where E is Gram equivalent weight
MOLARITY:
Number of grams moles of a solute dissolved per liter of solution is called Molarity.
It is denoted by M
Molarity = Wsolute/Msolute × 1/Vsovent (in lit)
Where M is Gram molecular weight
MOLALITY:
It is the number of mole of the substance dissolved in 1kg of the solvent it is denoted by (m).
Molality = Wsolute/Msolute × 1/Wsovent (in kg)
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EXPERIMENT-I
ESTIMATION OF FERROUS IRON BY DICHROMETRY
AIM: To estimate the amount of ferrous iron present of the whole solution with the help of
standard solution of potassium dichromate.
APPARATUS: Beaker, burette, pipette, conical flask, volumetric flask.
CHEMICALS: K2Cr2O7, diphenylamine, Conc. H2SO4, Distilled water.
THEROY AND PRINCIPLE:
Ferrous iron is oxidized to ferric iron by potassium dichromate in acid solution. The completion
of the oxidation of reaction is marked by the appearance of blue violet color of the
diphenylamine which is used as an internal indicator.
K2Cr2O7 +4H2SO4 → K2SO4 +Cr2 (SO4)3 +4H2O+3(O)
3[2FeSO4 +H2SO4+ (O) → Fe (SO4)3 +H2O]
K2Cr2O7 +6FeSO4 + 7H2SO4→K2SO4 + 3Fe2 (SO4)3 +Cr (SO4)3 + 7H2O
The equivalent weight of iron is its atomic weight i.e.55.86 since one equivalent of potassium
dichromate oxidizes one equivalent of iron.
PROCEDURE:
1) Preparation of standard potassium dichromate: weigh out accurately about 0.49gms of
potassium dichromate into a standard flask into a100 ml standard flask and dissolve the
solid in a small quantity of distilled water .make up the resulting solution with distilled
water up to the mark and shake the flask well for uniform concentration.
2) Preparation of acid mixture: Mix up 100 ml of phosphoric with 300ml of concentrated
H2S04 in a reagent bottle and stopper it.
3) Preparation of diphenylamine: Dissolve 1gm of diphenylamine in 100ml of concentrated
H2S04.
Standardization of ferrous iron:
Rinse the burette with K2Cr2O7 solution and take K2Cr2O7 solution up to the zero of the
burette. Pipette out 20ml of ferrous solution into a 250ml conical flask, add 5ml of acid
mixture and 2drops of diphenylamine indicator. Titrate the resulting solution with
potassium dichromate taken in the burette till blue violet color is obtained as end point.
Repeat the titration to get concurrent values.
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CALCULATIONS AND OBSERVATIONS:
S.No Fe+2 Solution(in ml) Burette reading
Initial final
Volume of k2cr2o7
Consumed (in ml)
Normality of K2Cr207 (N) = Wt .of K2Cr207 *10 / 49
Normality of ferrous iron (N2): N1V1 =N2V2
V1 = Volume of K2Cr207 (Titrevalue ….ml)
N2= Normality of K2Cr207
V2= Volume of ferrous iron
N2 =NIVI / V2 = Titer value* N1 / 20
RESULT: Amount of ferrous iron present in the given solution = ……………..gms/100ml.
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EXPERIMENT-2
Estimation of Hardness of water by EDTA method
AIM: To determine the total hardness, permanent hardness and temporary hardness of water
APPARATUS: Pipette,Burette,standard flask, conical flask,beaker,funnel.
CHEMICALS:Standard sample water, Buffer solution,EBT (Erichrome black –T)
indicator,distilled water EDTA(Ethylene diamine tetra acetic acetate)
PRINCIPLE: Calcium and magnesium ions which are present in standard water forms a weak
complex with EBT with wine red colour
Ca2+ / Mg2+ + EBT [Ca / Mg –EBT]
Unstable wine red complex
Then the solution is titrated against EDTA results in the formation of stable complex
changing colour from winered to blue
[Ca / Mg –EBT] + EDTA [Ca / Mg –EDTA] + EBT
(Wine red/unstable) (Stable) (Blue)
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Page | 10 B V Raju Institute of Technology (UGC Autonomous)
PROCEDURE:
STEP-1
STANDARDDISATION OF EDTA:
Pipette out 25 ml of standard hard water into a conical flask .To this add 5ml of buffer solution
followed by addition of 3 to 4 drops of EBT indicator. Then titrate against EDTA which is taken
in the burette. Continue the titration till wine red colour changes to blue colour. Repeat this
process until two concurrent values are obtained.
STEP-2
ESTIMATION OF TOTAL HARDNESS OF SAMPLE WATER
Take 50 ml of sample water into a conical flask.To this add 5ml of buffer solution
followed by addition of 3 to 4 drops EBT indicator.Then titrate against with EDTA which is
taken in burette.Continue the titration till winered colour to blue colour. Repeat this titration
until two concurrent values are obtained.
STEP-3
ESTIMATION OF PERMANENT HARDNESS OF SAMPLE WATER
Take 100ml of sample water in the beaker. Boil the water until its volume reduces to 50ml.Filter it into a standard volumetric flask and make the solution upto 100ml by adding distilled water. To this add 3 to 4 drops of EDTA indicator.Then titrate it against EDTA which is taken in the burette.continue the titration till wine red colour changes to blue colour. Repeat this process until two concurrent values are obtained. RESULT:
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EXPERIMENT-3
ESTIMATION OF PERCENTAGE OF COPPER IN BRASS
AIM: To determine the CU present in given brass sample by idometrically.
APPARATUS: Burette, Pipette, Conical Flask, Iodination flask, Standard Volumetric flask.
CHEMICALS: Standard Sodium thiosulphate (Na2S2O3), Hypo, Potassium iodide solution (KI),
CH3COOH, Starch, Dil HNO3, 0.1 N Hypo
PRINCIPLE: Cupric salt in neutral media when treated with KI forms a white PPT of Cuprous
iodide and decompose to liberate iodine, By estimating the liberated iodine CU can be
estimated.
𝐶𝑢 + 2𝐻𝑁𝑂3 → 𝐶𝑢(𝑁𝑂3)2 + 𝐻2 ↑
2𝐶𝑢(𝑁𝑂3)2 + 4𝐾𝐼 → 2𝐶𝑢𝐼2 + 4𝐾𝑁𝑂3
2𝐶𝑢𝐼2 → 𝐶𝑢2𝐼2 + 𝐼2
2𝑁𝑎2𝑆2𝑂3 + 𝐼2 → 𝑁𝑎2𝑆4𝑂6 + 2𝑁𝑎𝐼
2𝐶𝑢𝐼2 + 𝐼2 → 2𝑁𝑎2𝑆2𝑂3
PROCEDURE:
STEP I: DISSOLUTION OF BRASS:
Take the accurately weighted sample into 250ml beaker to that add 10ml of dil HNO3. Keep nit
on hot pan for heating purpose till the sample completely dissolve. Then transfer this solution
into clean 100ml standard volumetric flask by using funnel. Make up the solution up to 100ml
by adding distilled water.
STEP II: ESTIMATION OF CU IN BRASS:
Pipette out 200ml of solution from the standard volumetric flask. Add NH4OH till blue
color appears. Then add CH3COOH till its position in the solution becomes clear. To this add
20ml of KI and keep it in dark for 5mins. Then the color changes to thick brown color. After 5
min remove the Iodination flask from dark place and rinse the walls of the flask with
approximately 50ml of distilled water. Then titrate this against Hypo which is taken in burette.
The titration continues till the color changes to pale brown. Then add 3 drops of starch
indicator. Then color changes to black and titrate against Hypo until solution becomes clear. I.e.
Milky white.
RESULT:
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EXPERIMENT-4
ESTIMATION OF MNO2 IN PYROLUSITE
AIM: To estimate the amount of Manganese dioxide present in given pyrolusite sample by using
the standard potassium permanganate.
APPARATUS: Burette, Conical Flask, Funnel
CHEMICALS REQUIRED: Pyrolusite, 0.5 N Sodium oxalate, 0.3 N KMNO4, Dil H2SO4
PRINCIPLE: MNO2 present in pyrolusite is reduced by a known excess of oxalic acid in acidic
medium. Unreacted oxalic acid is treated against standard solution of KMNO4 till colour changes
to pink colour
Na2C2O4 + H2SO4 H2C2O4
Mno2 + H2C2O4+ H2SO4 MnSO4 + 2H2O + 2CO2
2KMnO4 + 3H2SO4 2MnSO4 + K2SO4 + 3H2O + 5 (O)
5 H2C2O4 + 5(O) 5H2O + 10 CO2
2KMnO4 + 3H2SO4 + 5H2C2O4 → 2MnSO4 + K2SO4 + 8H2O + 10 CO2
PROCEDURE: Weigh out the given sample and transfer the sample into conical flask. 40ml of
sodium oxalate followed by the addition of 50ml dil H2SO4 by keeping the funnel in the mouth
of conical flask. Then keep the conical flask along with funnel on hot pan for heating purpose
and continue till the black colored MNO2 particles disappeared in the solution and ring the
conical flask by adding 10 ml distilled water. Then titrate that solution against standard KMNO4
which is taken in burette and continue the titration till the change of colour from colourless to
pink. Then calculate the amount of oxalic acid consumed. From this it is possible to determine
MNO4 from pyrolusite.
RESULT:
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Page | 13 B V Raju Institute of Technology (UGC Autonomous)
EXPERIMENT-5
ESTIMATION OF IRON IN CEMENT BY COLORIMETICALLY
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EXPERIMENT-6
ESTIMATION OF COPPER BY COLORIMETRIC METHOD
AIM: Estimation of Copper by Colorimetry
APPARATUS: - Colorimeter, Test tubes, Burettes.
PRINCIPLE: - Colorimeter measures the optical density of an absorbing substance where optical
density (O.D) is defined as O.D = log 1oI
I
Where oI = Intensity of incident light
I = Intensity of transmitted light
As per beers law, optical density of an absorbing substance is related to the concentration by the
equation. . . .O D E C l
. ( . ). 2O D E l C
Where ‘C’ is the concentration of the substance, l is the path length, which represents the width
of the cell used and is constant for a given cell used, E is the molar absorption coefficient and is a
constant for given substance. Equation 2 may be written as O.D. C 3
Equation 3 represents the quantitative form of Beer’s law. if the optical density of a substance is
determined at varying concentration. A plot of O.D.vs C gives a straight line.
PROCEDURE:- take the sample solution of CuSo4 and prepare the following 10 sample solutions
in test tubes as 1 to 10
1. 1 ml 0.1 m CuSo4 + 9 ml Distilled water
2. 2 ml 0.1 m CuSo4 + 8 ml Distilled water
3. 3 ml 0.1 m CuSo4 + 7 ml Distilled water
4. 4 ml 0.1 m CuSo4 + 6 ml Distilled water
5. 5 ml 0.1 m CuSo4 + 5 ml Distilled water
6. 6 ml 0.1 m CuSo4 + 4 ml Distilled water
7. 7 ml 0.1 m CuSo4 + 3 ml Distilled water
8. 8 ml 0.1 m CuSo4 + 2 ml Distilled water
9. 9ml 0.1 m CuSo4 + 1 ml Distilled water
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10. 10 ml 0.1 m CuSo4 + 0 ml Distilled water
The ten sample solutions prepared above have a varying concern from 0.01m to 0.1m, choose the
filter in the colorimeter with maximum absorbance. Tabulate the result of filter and O.D with a
given CuSo4 sample solutions.
After selecting filter, determine the O.D. of the above mentioned ten sample solutions and tabulate
the results.
Observation:
Table-1
Filter No -Range (nm) Peak (nm) Optical Density(OD)
1
2
3
4
5
6
7
8
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Table-II Selected Filter--------------------
Sl.No Volume of
4CuSo (ml)
Volume of
2H O (ml)
Concentration of
4CuSo Optical Density
1
2
3
4
5
6
7
8
9
10
10
9
8
7
6
5
4
3
2
1
0
1
2
3
4
5
6
7
8
9
GRAPH: - Plot a graph of O.D Vs [CuSo4]. A straight line passing through origin is obtained
the slope of which gives El, E is the molar
absorption coefficient.
Slope 2 1
2 1
y y
x x
1
slopeslope El E
l
E mole cm
RESULT: - Amount of copper present in given CuSo4 solution is _________grams
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EXPERIMENT-7
CONDUCTOMETRIC TITRATION OF STRONG ACID Vs STRONG BASE
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EXPERIMENT-8
CONDUCTOMETRIC TITRATION OF MIXTURE OF ACIDS Vs STRONG BASE
AIM: - To determine the composition of mixture of acids by Conduct metrically
APPARATUS: - Conductivity meter, conductivity cells, Beakers, Pipette, Burette, conical flask
CHEMICALS: - acetic acid Solution (0.01N), NaOH Solution (0.1), HCl,
PRINCIPLE: - When mixture containing CH3COOH and HCl is titrated against an alkali strong acid
will be neutralized first, the neutralization of weak acid commences only after the completion of
strong acid. Then conductance titration curve will be marked by two breaks, the first one
corresponds to neutralization of HCl and second one to that of CH3COOH.
Let v1 & v2 ml be the volume of alkali corresponding to 1st and 2nd breaks, respectively.
V1ml of NaOH = HCl
(v1-v2) ml of NaOH = CH3COOH
PROCEDURE: -
Take 0.1 N NaOH solution and 0.01 N acetic acid Solution and 0.01 N HCl in a
beaker. Fill the micro burette with 0.1 N NaOH solution. Place the conductivity cell in distilled
water and adjust the display to PH 10 with calibration knob. Take a beaker and add 20 ml of
CH3COOH and 20 ml of HCl.Titrate this mixture against 0.1 N NaOH. Now measure initial
conductance of solution. Then 0.1 ml of 0.1 N NaOH is added every time from burette into the
solution and stirred well each time note down the conductance values till the conductance values
decreases and increases considerably.
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Graph: y
plot a graph between conductivity on
Y axis and volume of the base added on X axis
.
Vbase(in ml) x
N1V1=N2V2
Volume of NaOH Solution from graph V1 = -- ml
Normality of NaOH Solution N1= --- --N
Volume of mixture of acid solution V2= 20ml
Normality of mixture of acid solution N2 = -----N.
Normality of N2=-------------- N
RESULT: - The Strength of mixture of Acids is __________ N
Sl.No Volume of NaOH Conductivity (ohm-1)
1
2
3
.
.
.
.
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EXPERIMENT-9
POTENTIOMETRICTITRATION OF STRONG ACID vs. STRONG BASE
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Result:
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EXPERIMENT-10
POTENTIOMETRICTITRATION OF WEAK ACID vs. STRONG BASE
AIM: - To Determine the concentration of a weak acid by a Potentiometry titration given a
strong base of known concentration.
APPARATUS:- Potentiometer, Pt-electrode, Calomel electrode, Salt bridge, 150 ml beakers,
Stirrer, Pipette, Burette.
CHEMICALS: - 0.1m NaOH, 0.1m CH3COOH, Quinhydrone solid, KCl Solution.
PRINCIPLE: - The quinhydrone electrode is prepared by taking saturated solution of
quinhydrone in a known quantity of strong acid whose concentration is to be determined. This
electrode is combined with thecalomel electrode to make the cell. Pt, Hg,
Hg2Cl2(s)/Saturated//H+/QH2/Pt
In acid medium quinhydrone exist in two forms.
CH3COOH + NaOH → CH3COONa+H2O
As NaOH is added to a solution of H+ ions with quinhydrone the H+ ions are consumed steadily
and the relative concentration of QH2 and Q changes with the titration. At the end point where all
the ions are consumed, QH2 gets completely converted to Q. the electrode potential of the
electrodes is given as per the nearest equation.
Procedure: - Pipettes out 10 ml of the given CH3COOH solution into a clean100ml beaker add a
pinch of quinhydrone and stir it well to make a saturated solution of quinhydrone is H+. dip a
platinum electrode. Take a second beaker with saturated KCl solution in it. Dip the calomel
electrode in it. Connect two beakers with a salt bridge; connect the terminals of the potentiometer
with the two electrodes. Note the emf of the cell. Fill a burette with 0.1 NaOH, add 0.5ml of NaOH
into the beakers containing acid, stir well for equilibrium to establish. Note the emf of the cell
once again. The variation of emf by successive addition of 0.5 ml of NaOH. Each time will be about
10-20mv, as the endpoint approaches, the fall in the emf would increase from 10-20 mv to 40-50
mv. At this stage add NaOH in batches of 0.2 ml and note emf after each addition. At the end point
the emf falls suddenly by about 100-150 mv. Continue the titration with 0.2 ml of NaOH and note
5-6 emf values. Now the variation is emf gets smaller and takes 4-5 emf readings, after the
endpoint by adding batches of 1ml of NaOH each time, tabulate the results.
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Page | 27 B V Raju Institute of Technology (UGC Autonomous)
GRAPH: - Plot a graph of emf Vs volume of NaOH added and a second graph of /E V Vs Volume
of NaOH added. Note the point of Neutralization from both the graph and calculate the cone of
given CH3COOH using the concern of given NaOH as 0.1m
Sl.No Volume of Alkali (ml) Emf (mv)
1
2
3
.
.
.
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CALCULATION: -
CH3COOH NaOH
1 10V ml 2 _____V (From Graph)
1 ?N 2 0.1N
N1= Normality of CH3COOH N2 = Normality of NaOH
V1= Volume of CH3COOH V2 = Volume of NaOH
N1V1 = N2V2
N1 = N2V2/V1
Concentration of given CH3COOH (1N ) = ____N.
RESULT: - At the Neutralization point 10 ml of given CH3COOH= and concentration of given
CH3COOH =____
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EXPERIMENT-11
DETERMINATION OF VISCOCITY BY REDWOOD VISCOMETER
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Results:
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EXPERIMENT-12
DETERMINATION OF SURFACE TENSION OF LUBRICANTS
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Result:
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EXPERIMENT-13
Preparation of Aspirin
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Result:
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EXPERIMENT-14
Preparation of Thiokol rubber
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EXPERIMENT-15
ADSORPTION OF ACETIC ACID ON CHARCOAL
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Page | 39 B V Raju Institute of Technology (UGC Autonomous)
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