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F.E. SEM – II
(2020 – 21)
ENGINEERING CHEMISTRY – II
PRACTICALS
CONTENTS
Expt. Page
EXPERIMENTS Date Sign
No. No.
28/6/2021 2
Determination of Moisture content
1.
of Coal
28/6/2021 4
Determination of Ash Content of
2.
Coal
13/7/2021 6
3. Synthesis of Biodiesel
13/7/2021 9
4. Acid Value of Biodiesel
13/7/2021 13
5. Flame Photometry
28/6/2021 16
To determine the EMF of Cu-Zn
6.
System by Potentiometry.
REQUIREMENTS:
THEORY:
Moisture is an undesirable component of mined coal. It is bought and transported at the cost of
fuel. Moisture can be surface moisture which is lost on just air drying. However inherent moisture
is not lost by air drying.
PROCEDURE:
Note:
To get reproducible results, the sample should be powered and sieved to get uniform
sample. A care should be taken while weighing to ensure that no absorption of moisture
takes place.
CALCULATIONS:
REQUIREMENTS:
THEORY:
Ash is a useless, non-combustible matter, which reduces the calorific value of coal. Moreover, ash
causes the hindrance to the flow air and heat, thereby lowering the temperature. Also, it often
causes trouble during firing by forming clinkers, which blocks the interspaces of the grate, on
which coal is being burnt. This in-turn causes obstruction to air supply, thereby the burning of coal
becomes irregular. Hence, lower the ash content, better the quality of coal. The presence of ash
also increases transporting, handling and storage cost. It also involves additional cost in ash
disposal. The presence of ash also causes early ware of furnace wall, burning of apparatus and
feeding mechanism.
PROCEDURE:
1. The residual coal in the crucible from moisture experiment is heated without lid on a burner
for about 45 minutes.
2. The crucible is cooled and weighted.
3. Heating, cooling and weighing is repeated till a constant weight is obtained.
CALCULATIONS:
REQUIREMENTS:
• 250 ml beaker, and small watch glass • 125 ml ,250 ml conical flask and stopper
• Separating funnel, 250 ml • Stirring hot plate and magnetic stir bars
• Thermometer • Ethanol (anhydrous, 100%)
• 1 g potassium hydroxide • 100 g vegetable oil (Soyabean Oil)
THEORY:
Biodiesel is defined as the mixture of mono alkyl (generally methyl and ethyl) esters of long chain
fatty acids derived from vegetable oils or animal fats, for use in compression-ignition (diesel)
engines.
The process of making biodiesel from vegetable oil is called transesterification. This is a chemical
reaction in which 1 mole of triglycerides (vegetable oil or animal fats) reacts with 3 moles of
alcohol to produce 3 moles of alkyl esters (biodiesel) and 1 mole of glycerol, a co-product. This is
a reversible, equilibrium reaction and requires excess alcohol to push it toward the products side.
Usually, 6 moles of alcohol are used per 1 mole of triglycerides. Le Chatelier's principle explains
this behaviour.
Typically, a strong base such as sodium hydroxide (NaOH) or potassium hydroxide (KOH) is used
as the catalyst.
PROCEDURE:
1. Calculate the molecular weight of ethanol X g/mol.
2. Since we are using 100 g of oil (M W = 878 g/mol), we can use the following relationship
to calculate the ethanol needed for a 6:1 ratio of ethanol moles to triglyceride moles:
877 g of oil = 6 X g of ethanol
3. Weigh out 1 g of potassium hydroxide into a 125 ml Conical flask. Into this same
flask add the calculated amount ethanol.
4. Add a magnetic stir bar, cover with a watch glass, and place on a stirring hot plate. Mix
until the KOH is completely dissolved. Set this aside.
5. Weigh an empty 250 ml conical flask. Into this same flask weigh out about 100 g of
oil and record the weight W1. Add a stir bar, put on a hot plate, and heat to around
60 °C.
6. Next, add the alcohol/catalyst mixture to the oil in the flask and cover with a watch glass
to keep the alcohol vapours from escaping. Stir this mixture at a moderate level for 60
minutes while holding the temperature at 60 °C.
7. Transfer the mixture to a separating funnel and allow it to settle for 20 minutes.
8. Remove the glycerine (lower) layer. The upper phase is the biodiesel.
Note: If there is no phase separation after 5 to 10 minutes, it can be forced by the addition of
water. Return the mixture to the 250 ml conical flask, and while stirring, add 15 ml of water
and continue to stir for about 10 seconds. Then, return the mixture to the separating funnel.
This action will concentrate the polar molecules of water, ethanol and glycerol and allow them
to settle along with a good portion of the soap.
9. Weigh a clean 250 ml beaker and record the weight. Next weigh the clean biodiesel
and record that weight W2 to be used for the yield calculation.
ENGINEERING CHEMISTRY - TSEC/2020-21
II
REACTIONS:
% Yield = 87.64%
= 924 X 100
878 + 3(46)
= 90.94%
RESULT:
REQUIREMENTS:
N /10 KOH, Ethyl alcohol, Phenolphthalein indicator, Burette, Round bottom flask, Water
condenser, biodiesel sample, etc.
THEORY:
The acid value of Biodiesel is defined as the number of milligrams of potassium hydroxide
In good biodiesel the acid value should be very low (< 0.1). Increase in acid value should be
taken as an indicator of oxidation of the oil which may lead to corrosion of machine parts.
The acid value of biodiesel may vary from 0.2 to 50 & it shows the extent of hydrolysis of
PROCEDURE:
2. Add 2 drops of Phenolphthalein & titrate against KOH solution. End point is from
colourless to pink.
1. Weigh out accurately about W gm of biodiesel under test into a 250 ml conical flask
& add 25 ml of neutral alcohol. Heat the flask with air condenser over the water
bath for about 30 min. Cool the flask & the contents to room temperature & add a
2. Titrate with standard N/10 KOH solution until a faint permanent pink colour
REACTIONS:
CALCULATIONS:
CALCULATIONS:
neutralization Therefore,
= 56 X 2.6_X 0.1
2.5
= 5.24
RESULT :
AIM: To estimate the sodium content in the given sample of water by flame photometry.
PRINCIPLE:
Emission of characteristic radiation by an element and the correlation of the emission intensity with the
concentration of the element form the basis of flame photometry.
When a solution containing the sample element or ion is aspirated into the flame, a series of changes
take place at the flame. First the solvent gets evaporated leaving behind the salt in the flame. The salt then
gets evaporated into vapors of the salt, which further undergo dissociation into the constituent atoms. Some
of the metal atoms formed in the flame may absorb heat energy from the flame and get electronically excited
and come back to ground state by emitting the energy (difference between the excited and ground state), in
the form light radiation. The intensity of the light radiation emitted is proportional to the number of atoms in
the flame or the concentration of the solution fed into the flame. Thus concentration of the solution is related
to the intensity of the emitted radiation. By measuring the intensity of the emitted radiation by a suitable
detector device, the concentration can be determined. As different metals emit their characteristic radiations
at different wave lengths, they do not interfere with each other, even when they are present together. The
different radiations emitted by the different metal atoms can be resolved by using a dispersive unit, detected
and measure for analysis.
The sequence of changes taking place in the flame, when metal salt solution is aspirated may be
summarized as follows:
The intensity of the emitted radiation, measured as detector response is related to the concentration
by an expression similar to Beer’s relation,
E=kαc
where E is the detector response, k is a constant, α is the efficiency of atomic excitation and c is the
concentration of the solution.
The qualitative analysis by flame photometry can be carried out by calibration curve method. For
this purpose, a series of standard solutions of the analyte metal are taken, aspirated into the flame and the
emission of each solution is measured in a flame photometry. Then the calibration curve is obtained by
plotting the emission intensity against the concentration of the standard solutions. The sample solution is
properly diluted so that its emission is in a range to the standard, and its emission is measured. Form the
calibration curve, the concentration of the sample solution can be determined.
PROCEDURE:
Pipette out 5, 10, 15 and 20 ml of the standard NaCl solution containing 0.1 mg of Na per ml of solution into
4 different 100 ml standard flasks. Make the solution up to the mark with distilled water and shake for
uniform concentration. Take the first standard solution in a small beaker and aspirate into the flame of flame
photometer. The flame emission intensity of the standard is measured by flame photometer using sodium
filter into the photometer. The same is repeated for all standard solutions with distilled water being sprayed
to flame in between the trials. Plot the calibration curve by plotting emission response along Y-axis &
concentration of solution along X-axis.
Then aspirated the given sample of water into the flame and note down the value of emission response. From
the calibration curve compute the concentration of Na in the water sample.
10 10 15
15 15 20
20 20 24
Unknown 8 11
GRAPH:
Emission
Response
Concentration (Unknown)
THEORY: In the Daniel cell, a piece of zinc metal is placed in a solution of zinc sulfate in one
container, and a piece of copper metal is placed in a solution of copper(II) sulfate in another
container. These strips of metal are called the cell’s electrodes. The electrodes act as a terminal, or
a holding place, for electrons. A wire connects the electrodes, but nothing happens until you put a
salt bridge between the two containers.
The salt bridge, normally a strip of filter paper soaked in KCl, provides a way for ions to move
from one container to the other to keep the solutions electrically neutral. With the salt bridge in
place, electrons can start to flow. Zinc is being oxidised, releasing electrons that flow through the
wire to the copper electrode, where they’re available for the Cu 2+ ions to use in forming copper
metal. Copper ions from the copper(II) sulfate solution are being deposited on the copper
electrode, while the zinc electrode is being consumed. The cations in the salt bridge migrate to the
container containing the copper electrode to replace the copper ions being consumed, while the
anions in the salt bridge migrate toward the zinc side, where they keep the solution containing the
newly formed Zn2+ cations electrically neutral.
The zinc electrode is called the anode, the electrode at which oxidation takes place, and is labelled
with a “–” sign.
The copper electrode is called the cathode, the electrode at which reduction takes place, and is
labelled with a “+” sign.
This cell will produce a little over one volt. You can get just a little more voltage if you make the
solutions that the electrodes are in very concentrated.
MATERIALS REQUIRED:
1. 100ml beakers
2. Copper and Zinc rods.
3. 1.0 M zinc sulfate, 1.0 M copper sulfate, 0.1 M zinc sulfate, 0.1 M copper sulfate
4. 0.5 M Potassium Chloride Solution
5. Filter paper for salt bridge
6. Measuring cylinders
7. Multimeters / Potentiometer.
8. Connecting wires
9. Crocodile clips
1.
Place 1.0 M ZnSO4 (Zinc Sulphate) solution in a 100 cm3 beaker and a 1.0 M CuSO4
(Copper sulfate) in another beaker of the same size.
2.
A clean strip of zinc was placed into the zinc solution and a clean strip of copper was
placed into the copper solution. The electrodes were rinsed with distilled water thoroughly
before use.
3.
Connect the Zinc electrode to negative terminal of potentiometer and connect Copper
electrode to positive terminal of potentiometer.
4.
The half cells were connected with a length of filter paper soaked in 0.5 M potassium
chloride solution.
5.
Electrons flowed from the zinc electrode to the copper electrode because of the reactions
occurring in the half-cells: Zn → Zn2+ + 2e- and Cu2+ + 2e- → Cu.
6.
The overall reaction for the cell is:
Cu2+ + Zn → Cu + Zn2+.
The voltage of this cell is measured. Also, the voltages of a Daniel cell with 0.1 M ZnSO 4
and 1.0M CuSO4, and with 1.0 M ZnSO4 and 0.1 M CuSO4 is measured.
Concentration of Concentration of
Measured Voltage (V) Theoretical Voltage(V)
ZnSO4 CuSO4
1.10 1.10
1M 1M
1.119 1.13
0.1 M 1M
1.028 1.07
1M 0.1 M
1.046 1.10
0.1 M 0.1 M
CALCULATIONS: