Lab Manual
Lab Manual
Lab Manual
LAB MANUAL
ENGINEERING CHEMISTRY
100012
Year 2021-22
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
To provide students with practical knowledge of quantitative analysis of materials by classical and
instrumental methods for developing experimental skills in building technical competence.
List of Experiments
Subject: Engineering Chemistry laboratory (Common to B.TECH. I st year-all branch)
Paper code 100012
NOTE: At least 10 of the following core experiments must be performed during the session.
10 Determination of Moisture content, volatile matter content, Ash content and fixed
Carbon of a given sample of coal by proximate analysis.
11 Preparation of phenol formaldehyde resin by condensation polymerization.
EXPERIMENT NO: 1
Aim: To determine the total hardness of given water sample by Complexometric titration.
Apparatus: Pipette, Burette, standard flask, conical flask, beaker, funnel.
Chemicals: Standard sample water, Buffer solution (10pH), EBT (Eriochrome black –T) indicator,
distilled water EDTA (Ethylene di-amine tetra acetic acetate), sample hard water.
Theory: The property of water which restricts or checks the lather formation with soap is called hardness.
In other words, the presence of multivalent cations, mostly calcium and magnesium ions, in water is referred
to as hardness of water. Hardness is of two types: Temporary or carbonate hardness which can be removed
by boiling and Permanent or Non carbonate hardness which cannot be removed by boiling. The hardness is
usually expressed in parts of CaCO3 equivalent or calcium and magnesium salts per million parts of water i.e
in ppm. The hardness of water can be determined by Complexometric titration using Ethylene di-amine tetra
acetic acid (EDTA). EDTA in the form of its di-sodium salt forms complex with Ca2+ and Mg2+ ions of
water sample. When Eriochrome Black T (EBT) indicator is added to the hard water at pH around 9–10, it
gives wine red colored unstable complex with Ca2+ and Mg2+ ions of water sample.
Ca2+ / Mg2+ + EBT [Ca / Mg –EBT]
Unstable wine red complex
When this wine red colored complex is titrated against EDTA solution of known strength the Ca2+ and
Mg2+ ions forms stable metal complex with EDTA and color changes from wine red to blue (color of EBT
indicator) at the end point. So titration at pH about 9–10 using EBT indicator gives the total amount of Ca2+
and Mg2+ ions in the water sample.
Procedure:
Step-1: Standardization of EDTA:
Pipette out10 ml of standard hard water into a conical flask .To this add 2ml of buffer solution
followed by addition of 1 to 2 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 wine red colour to blue colour. Repeat this titration until two concurrent
values are obtained.
Obervation table:
16.2
16.2
Calculation:
Precautions:
i) All the glass apparatus should be washed thoroughly with distilled water before use.
ii) The burette and pipette should be rinsed with solution to be taken in it.
iii) There should not be any leakage in the burette. iv) All the solution should be freshly prepared.
iv) Same amount of indicator should be added each time.
v) pH of the solution should be maintained during titration.
vi) Shaking should be proper during titration.
vii) The titration flask should be placed on white paper or board to identify properly the colour
change at the end point.
viii) All reagents should be used freshly prepared.
---------------------------------
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
EXPERIMENT-2
Aim: To determine permanent hardness and temporary hardness of given water sample by
Complexometric titration.
Apparatus: Pipette, Burette, standard flask, conical flask, beaker, funnel.
Chemicals: Standard sample water, Buffer solution(10pH), EBT (Eriochrome black –T) indicator,
distilled water, EDTA(Ethylene di-amine tetra acetic acetate) sample hard water.
Theory: The property of water which restricts or checks the lather formation with soap is called hardness.
In other words, the presence of multivalent cations, mostly calcium and magnesium ions, in water is referred
to as hardness of water. Hardness is of two types: Temporary or carbonate hardness which can be removed
by boiling and Permanent or Non carbonate hardness which cannot be removed by boiling. The hardness is
usually expressed in parts of CaCO3 equivalent or calcium and magnesium salts per million parts of water
i.e. in ppm. The hardness of water can be determined by Complexometric titration using Ethylene di-amine
tetra acetic acid (EDTA). EDTA in the form of its di-sodium salt forms complex with Ca2+ and Mg2+ ions
of water sample. When Eriochrome Black T (EBT) indicator is added to the hard water at pH around 9–10, it
gives wine red colored unstable complex with Ca2+ and Mg2+ ions of water sample.
Ca2+ / Mg2+ + EBT [Ca / Mg –EBT]
Unstable wine red complex
When this wine red colored complex is titrated against EDTA solution of known strength the Ca2+ and
Mg2+ ions forms stable metal complex with EDTA and color changes from wine red to blue (color of EBT
indicator) at the end point. So titration at pH about 9–10 using EBT indicator gives the total amount of Ca2+
and Mg2+ ions in the water sample.
Procedure:
Step-1: Standardization of EDTA:
Pipette out10 ml of standard hard water into a conical flask .To this add 2ml of buffer solution
followed by addition of 1 to 2 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 10 ml of sample water into a conical flask. To this add 2ml of buffer solution followed by
addition of 1to 2 drops EBT indicator. Then titrate against with EDTA which is taken in burette.
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Continue the titration till wine red colour to blue colour. Repeat this titration until two concurrent
values are obtained.
Step-3 : Estimation of permanent hardness of sample water
Take 25ml of sample water in the beaker. Boil the water until its volume reduces to 15ml.Take 10
of this boiled and cool water in conical flask. To this add 1 to 2drops of EBT indicator. Then titrate
it against EDTA which is taken in burette. Continue the titration till wine red colour changes to blue
colour. Repeat this process until two concurrent values are obtained.
Observation table:
Calculation:
Volume of EDTA x 1000
Total Hardness =
(ppm) Volume of water sample taken
Result: The permanent hardness and temporary hardness of given water sample is ------- ------- ppm
respectively.
Precautions:
i) All the glass apparatus should be washed thoroughly with distilled water before use.
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
ii) The burette and pipette should be rinsed with solution to be taken in it.
iii) There should not be any leakage in the burette. iv) All the solution should be freshly prepared.
iv) Same amount of indicator should be added each time.
v) pH of the solution should be maintained during titration.
vi) Shaking should be proper during titration.
vii) The titration flask should be placed on white paper or board to identify properly the colour
change at the end point.
viii) All reagents should be used freshly prepared.
---------------------------------
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
EXPERIMENT-3
Aim: To determine carbonate, bicarbonate and hydroxide alkalinity of given water sample by
neutralization titration.
Apparatus: Burette, Pipette, Conical flask, Dropper, measuring cylinder, Beaker etc.
Chemicals: 0.02 N HCl, phenolphthalein indicator & methyl orange indicator.
Theory: Due to the presence of those minerals, which increase the concentration of OH¯ ions in
water, the pH of water increases & it becomes alkaline. Alkalinity is divisible into bicarbonate
alkalinity, carbonate alkalinity & hydroxide alkalinity. In most waters bicarbonates (HCO3-) and
carbonates (CO3-2) are the major bases.
Alkalinity refers to the capability of water to neutralize acid. Alkalinity is often related to hardness
because the main source of alkalinity is usually from carbonate rocks (limestone), which are mostly
CaCO3. If CaCO3 actually accounts for most of the alkalinity, hardness in CaCO3 is equal to
alkalinity.
The above alkalinities can be determined volumetrically by titrating water sample against standard
acid using methyl orange and phenolphthalein indicators.
Detected by
Phenolphthalein Indicator
OH¯ + H+ H2O (one step neutralization, P =M)
Detected by
Methyl orange Indicator
HCO3¯ + H+ H2 CO3 (one step neutralization, M)
Detected by
Phenolphthalein Indicator
CO32 ― + H+ H CO3¯ (first step)
Detected by
Methyl orange Indicator (Two step neutralization, 2P)
HCO3¯ + H+ H2 CO3 (second step)
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Procedure:
Determination of alkalinity
Pipette out 10 ml of filtered water sample in a conical flask & add 1-2 drops of alcoholic
phenolphthalein indicator to it. If the solution turns pink then titrate it with 0.02N HCl until
colourless. Let this burette reading be V1. To the same solution or to the solution, which remains
colourless even after adding phenolphthalein indicator, add 1-2 drops of methyl orange indicator. If
the solution becomes yellow then continue titration till orange pink colour is obtained at the end
point. Let this burette reading be V2 from the beginning and is called methyl orange end point.
Repeat the titration for two more times & find the constant burette reading.
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Reference table:
Observation table:
S.No. Volume of Water Volume of HCl required (mL)till Volume of HCl required (mL)till
Sample Taken (mL) phenolphthalein end point V1 methyl orange end point V2
1 10 ml 0.4 2.3
2 0.4 2.1
3 0.4 2.1
4
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Calculations:
V1 x Normality of HCl x 50000
Phenolphthalein alkalinity (P) =
(ppm) Volume of water sample taken
Result: The bicarbonate, carbonate and hydroxide alkalinity of given water sample are -------, ---------- &
-------- Respectively.
Precautions:
All the glass apparatus should be washed thoroughly with distilled water before use
The burette and pipette should be rinsed with solution to be taken in it.
There should not be any leakage in the burette.
The conical flask should be placed on white paper or board to identify the colour change at the end
point.
The same amount of indicator should be used in all titrations.
The reaction mixture should be shaken properly during titrations.
Titration is to be carried out at room temperature.
The end point of the titration should be noted carefully.
---------------------------------
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
EXPERIMENT-4
Aim: To determine percentage of iron ( Fe II) in given iron alloy solution in which 3gms of iron
alloy dissolved in one litre of solution by Redox titration
Apparatus: Pipette, Burette, conical flask, beaker, funnel.
Chemicals: Standard FAS (Mohr’s salt) solution, KMnO4 solution, iron alloy solution.
Theory: Titrations in which a reducing agent is titrated against an oxidizing agent or vice versa are
called Redox titration. In a redox reaction if one substance is oxidized the other is reduced.
Oxidation is defined as the process in which loss of electron from the element takes place and
reduction is a process where electrons are accepted by the element or the ion. The reagent which
undergoes reduction is an oxidizing agent and the reagent which undergoes oxidation is a reducing
agent. The oxidation and reduction are complementary to one another and takes place
simultaneously. The equivalent weight of an oxidizing and reducing agent can be obtained by
dividing molecular weight of the compound by the total number of electrons that are gained or lost
in a reaction per molecule of the substance.
Fe 2+ – e = Fe 3+
In this redox titration under experiment KMnO4 oxidizes ferrous ion of the salt to ferric ion in
acidic medium and itself reduces to colorless manganous (Mn 2+) ion.
Fe 2+ – e Fe 3+ x 5
___________________________________________
MnO4 − + 8H+ + 5 Fe2+ Mn2+ + 5 Fe3+ + 4 H2O (Ionic equation)
As the change in colour in acid – base indicator depends on the pH of the reaction mixture, the
change in colour of the indicator in redox titration depends upon the electrode potential of the
system. Therefore, a redox indicator has to be chosen in such a way that its potential lies within that
of the system. In this titration, KMnO4, the oxidizing agent is the self indicator as it is strongly
coloured (purple) and decolorizes after reduction. Potassium permanganate is purple in its oxidized
form (MnO4 – ) but its reduced form (Mn2+ ) is colorless in acidic medium.
As, the titration proceeds, the MnO4– will converted to Mn2+ and simultaneously Fe2+will converted
to Fe3+. When whole of the reducing agent (Fe2+ ) will consumed, the oxidizing agent (MnO4–)
cannot be reduced, then the addition even one drop of KMnO4 solution given its colour to the
solution. This indicates the end point of the titration.
Procedure:
1. Primary standard FAS solution was provided.
2. Standardization of KMnO4 solution by standard FAS solution: Pipette out 10 mL of standard
FAS solution in which dilute H2SO4 (1:8 V/V) is already added. Titrate with standard KMnO4
solution of known strength from the burette with constant stirring till the first permanent pink color
develops in the solution. Repeat this process until two concurrent values are obtained.
3. Estimation of Fe (II) in the given alloy solution: Pipette out 10 ml of unknown Fe(II) alloy
solution in a 100 ml conical flask, in which dilute H2SO4 (1:8 V/V) is already added. Titrate with
standard KMnO4 solution till the first permanent pink color develops throughout the whole mass of
the solution. Repeat this process until two concurrent values are obtained.
Observations Table 1:
FAS vs. KMnO4
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Observations Table 2:
Precaution:
i) All the glass apparatus should be washed thoroughly with distilled water before use.
ii) Burette and pipette should be rinsed with the solution to be taken in it.
iii) There should not be any leakage in the burette.
iv) KMnO4 solution should be kept in dark.
v) KMnO4 solution should not be filtered through filter paper, it should be taken by
decantation.
vi) Freshly prepared KMnO4 should be used.
vii) H2SO4 should be added in excess otherwise brown precipitate of MnO2 may appear.
viii) The conical flask should be placed on white paper or board to identify properly the color
change at the end point.
---------------------------------
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Experiment No.5
Aim: To determine percentage of chromium in given chromium alloy solution in which 3gms of
chromium alloy dissolved in one liter of solution by Redox titration
Theory:-
It is redox reaction in which chromium alloy solution alloy is mixed with excess of FAS and
reduced rapidly to green chromium (III) in a acidic medium at ordinary temperature and FAS
oxidized to Fe3+
The remaining FAS is back titrated with KMno4 and oxidized to Fe3+ ion and KMno4 reduced to
colourless manganous ions.
Procedure:-
Fill the burette with standard KMno4 Solution. Now pipette out 10 m1 of Chromium alloy solution
in a conical flask. To this add 20 ml of FAS solution with the help of pipette. Immediately after the
addition of FAS a greenish colour is formed. Now titrate this solution with standard KMno4
Solution, filled in the burette, until the greenish colour is converted into pink colour. Repeat this
entire process until two concordant reading are obtained.
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Observation Table:
Calculation:-
N1 V1 = N2V2
N2=N1V1/V2
Result:-
The % of Chromium present in a given Chromium alloy Solution is ---------%.
Precautions:
i) All the glass apparatus should be washed thoroughly with distilled water before use.
ii) Burette and pipette should be rinsed with the solution to be taken in it.
iii) There should not be any leakage in the burette.
iv) KMnO4 solution should be kept in dark.
v) KMnO4 solution should not be filtered through filter paper, it should be taken by
decantation.
vi) Freshly prepared KMnO4 should be used.
vii) H2SO4 should be added in excess otherwise brown precipitate of MnO2 may appear.
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
viii) The conical flask should be placed on white paper or board to identify properly the color
change at the end point.
------------------------------
Experiment No.6
Aim: To determine the percentage of Copper in a given Copper alloy solution in which 3gms of
Copper alloy dissolved in one litre of solution by iodometric titration.
Procedure:-
1. Fill a clean burette with Na2S2O3 solution
2. Take 10 ml of Copper alloy solution in a conical flask.
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
3. Add 1 ml of 10% KI solution and cover the flask and swirl the solution.
4. Titrate the copper alloy solution until brown colour fades.
5. Add at this stage 1ml of starch solution, blue colour appears.
6. Continue the addition of hypo, until blue colour commences to disappear.
7. Repeat the titration to get at least two concordant reading.
Observation Table:-
S.No. Volume of Alloy Burette Reading Volume of
Na2S2O3Used
Calculation:- N1 V1 = N2V2
N2=N1V1/V2
Percentage of copper =
Precautions:
i) All the glass apparatus should be washed thoroughly with distilled water before use.
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
ii) Burette and pipette should be rinsed with the solution to be taken in it.
iii) There should not be any leakage in the burette.
iv) Freshly prepared starch indicator should be used .
v) starch indicator should be used near the end point.
vi) The conical flask should be placed on white paper or board to identify properly the color
change at the end point.
Experiment No.7
Aim: Determine the viscosity of given lubricating oil by Redwood viscometer No.1 at room
temperature and at 60˚C.
Requirement: Red Wood viscometer No.1, stop watch, lubricating oil, thermometer.
Theory: The viscosity of lubricating oil can be determined by measuring the rate of flow oil
through a capillary tube kept at a uniform temperature. But in case of lubricating oil specific
viscosity is generally determined by measuring the time taken for a given quantity of oil to flow
through an orifice or jet of standard dimensions. Under standard conditions, three types of
standared viscometer namely Redwood, Engler and saybolt viscometer are in common use.
The redwood viscometer measure viscosity in empirical units not in absolute unit. There are two
types of Redwood viscometer i.e. Redwood viscometer No.1 and Redwood viscometer No.2.
Redwood viscometer No.1 will correctly indicate the viscosity for a liquid having flow time
between 30seconds to 2000seconds.if the flow time measured with this apparatus for any oil
exceeds 2000 seconds the test should be repeated with Redwood viscometer No.2which will give
the correct value of viscosity for such highly discus oil. The two viscometers Redwood viscometer
No.1 and Redwood viscometer No.2 are identical in principle, shape and mode of testing. They
differ only in dimensions of orifice.
Procedure:
1. Clean the viscometer cup and properly dry it to remove any trace of the solvent.
2. Level the viscometer with help of leveling screw.
3. Place the ball valve on the jet to close it and pour the test oil in to the cup up to tip of
indicator.
4. Place a clean dry kohlrausch flask or beaker immediately below and directly in line with
discharging jet.
5. Insert a thermometer and stirrer in the cup and cover it with a lid.
6. Lift the ball valve and start the stop watch. Oil from the jet flows in to the flask.
7. Stop the stop watch when a lower meniscus of oil reaches the 50 ml mark on the neck of the
receiving flask (replace the ball valve in position immediately so as to prevent overflow).
8. Record the time taken for 50 ml of oil to collect in flask.
9. Repeat the experiment to get the reproducible results and report the mean value in second.
10. Refill the oil cup to the indicator tip of oil cup.
11. Fill the outer bath with water to determining the viscosity at 60˚C and below, for higher
temperature, the bath is filled with oil having suitable visibility at the test temperature.
12. Connect the heater switch to the viscometer. Heat the water filled in the bath slowly with
constant stirring. When the oil in cup attains a desired temperature stop the heating.
13. Repeat the experiment at 60˚C and note the time taken for 50 ml of oil to collect in flack.
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Observation table:
Experiment No.8
Aim: - Determination of flash point and fire point of given lubricating oil by Pensky-Marten’s
closed cup flash point apparatus.
Theory:-
The Flash Point of oil may be defined as the minimum temperature to which it must be heated to
give off sufficient vapours to ignite momentarily or less than 5 seconds when a flame of standard
dimensions (Aprrox. 4 mm) is brought near the surface of the sample for a prescribed rate in an
apparatus of specified dimensions. This is detected by the appearance of momentary flash upon the
application of small flame over the surface of oil.
The Flash Point is defined as closed cup or open cup flashpoint accordingly as the apparatus for the
determination of flash point of sample is provided with a cover to cover the sample cup or not.
Whereas the Fire Point of oil may be defined as the minimum temperature to which it must be
heated to give off sufficient vapours to ignite for more than 5 seconds when a flame of standard
dimensions (Aprrox. 4 mm) is brought near the surface of the sample for a prescribed rate in an
apparatus of specified dimensions. The mechanism of the appearance of the flash can be explained
in the following manner. Every flammable liquid has a vapour pressure, which is a function of the
liquid’s temperature. As the temperature increase, the vapour pressure increases, as the vapour
pressure increases, the concentration of evaporated flammable liquid in the air increases. Hence,
temperature determines the concentration of its vapours in the air to sustain combustion. The flash
point of a flammable liquid is the lowest temperature at which there can be enough flammable
vapour to ignite, when an ignition source is applied. Oil containing minute quantities of volatile
organic substances is liable to flash below the true flash point of the oil. Although a small flash may
be observed in such cases, it should not be confused with the true flashpoint, since its intensity does
not increase with increase in temperature, as occurred when the true flash point is reached.
Importance of flash point from view of lubricants:
Good lubricating oil should not volatilize under the working temperatures. Even if some
volatilization takes place, the vapour formed should not form inflammable mixture with air under
the condition of lubrication. From this point of view, the flash point of lubricating oil is of vital
importance. Lubricating oil selected for the job should have a flash point which is reasonably
above its working temperature. This insures the safety against the fire hazards during the storage,
transport and use of the lubricating oil. This test is immense importance for illuminating and
lubricating Oils. This helps in detecting the highly volatile constituents of the oils. If they are highly
volatile at ordinary temperature, the issuing vapors may cause fire hazards. So to ensure safety,
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
certain minimum temperatures are laid down for fuels and Lubricating Oils below which they
should not give off adequate vapors to make them burn.
PROCEDURE:
1. The cup and its accessories are well cleaned and dried before the test is started.
2. Now the cup is filled with the oil to be tested up to the level indicated by the filling
mark and covered with the lid.
3. The stirring device, the thermometer and flame exposure device is fixed on the top of the
cover.
4. The cup is now set in the apparatus properly and the thermometer inserted
5. The test flame is lighted and adjusted until it is the size of a bead (4mm in diameter).
6. The apparatus is heated so that the heating rate is maintained, with the help of a rheostat, at
5-6 0C per minute and stirring rate at 1 to 2 rps.
7. Once the heating started, the test flames is applied after each 2˚C rise of temperature nearer
to the sample in the cup by opening the shutter and check the appearance of the flash. On
observing a flash, stop the heating process and allow the temperature to decrease. Check the
occurrence of a flash at every 1˚C drop in temperature.
8. Record the lowest temperature at which the flash is observed as the flash point of the
sample.
9. The oil sample is further heated at a rate of about 1˚C/minute and the test flames is applied
after each 1˚C rise of temperature of oil. The temperature, at which the vapours of oil sample
give a clear and distinct blue flame, is recorded as fire point.
Result:
1. The flash point of given oil sample is ………… ˚C
2. The fire point of given oil sample is ………… ˚C
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Precaution:
Experiment No.9
Aim: Determination of flash and fire points of a lubricating oil by Cleveland’s open cup flash point
apparatus.
Theory: The Flash Point of oil may be defined as the minimum temperature to which it must be
heated to give off sufficient vapors to ignite momentarily or less than 5 seconds when a flame of
standard dimensions (Aprrox. 4 mm) is brought near the surface of the sample for a prescribed rate
in an apparatus of specified dimensions. This is detected by the appearance of momentary flash
upon the application of small flame over the surface of oil. The Flash Point is defined as closed cup
or open cup flash point accordingly as the apparatus for the determination of flash point of sample
is provided with a cover to cover the sample cup or not.
Whereas the Fire Point of oil may be defined as the minimum temperature to which it must be
heated to give off sufficient vapour to ignite for more than 5 seconds when a flame of standard
dimensions (Aprrox. 4 mm) is brought near the surface of the sample for a prescribed rate in an
apparatus of specified dimensions.
The mechanism of the appearance of the flash can be explained in the following manner. Every
flammable liquid has a vapour pressure, which is a function of the liquid’s temperature. As the
temperature increase, the vapour pressure increases, as the vapour pressure increases, the
concentration of evaporated flammable liquid in the air increases. Hence, temperature determines
the concentration of its vapour in the air to sustain combustion. The flash point of a flammable
liquid is the lowest temperature at which there can be enough flammable vapour to ignite, when an
ignition source is applied. Oil containing minute quantities of volatile organic substances is liable to
flash below the true flash point of the oil. Although a small flash may be observed in such cases, it
should not be confused with the true flash point, since its intensity does not increase with increase
in temperature, as occurred when the true flash point is reached.
Importance of flash point from view of lubricants:
Good lubricating oil should not volatilize under the working temperatures. Even if some
volatilization takes place, the vapour formed should not form inflammable mixture with air under
the condition of lubrication. From this point of view, the flash point of lubricating oil is of vital
importance. Lubricating oil selected for the job should have a flash point which is reasonably above
its working temperature. This insures the safety against the fire hazards during the storage, transport
and use of the lubricating oil. This test is immense importance for illuminating and lubricating Oils.
This helps in detecting the highly volatile constituents of the oils. If they are highly volatile at
ordinary temperature, the issuing vapors may cause fire hazards. So to ensure safety, certain
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
minimum temperatures are laid down for fuels and Lubricating Oils below which they should not
give off adequate vapors to make them burn.
Description of apparatus:
The apparatus consists of a test cup made of without any lid and is equipped with a handle. The cup
is supported by a metal plate known as heating plate. The cup may be heated by an electric heater
mounted below the cup in the apparatus itself the metal plate has an extension for mounting the test
flame and the thermometer support. The test flame is mounted in such a manner as to permit
automatic duplication of the sweep of the test flame over the sample cup. The size of the flame can
be adjusted with respect to the dimension of metal bead (4 mm).
Procedure:
1. The apparatus is thoroughly cleaned and the thermometer is suspended in such a way so
that the bottom of the thermometer bulb just above the bottom of sample cup.
2. The cup is now filled with sample up to the filling mark grooved on the inner side of the
cup taking care that the surface of the sample is free from bubbles and there is no oil above
the filling mark.
3. The test flame is adjusted to have a flame diameter of about 4 mm.
4. Now move the test flame over the sample cup and check the appearance of flash over the
sample inside the cup.
5. If no flash observed, increase the temperature of the sample taken and take a flame over the
cup after every 2 ˚C increases. On observing a flash, stop the heating process and allow the
temperature to decrease.
6. Check the occurrence of a flash at every 1 ˚C drop in temperature. Record the lowest
temperature at which the flash is observed as the flash point of the sample.
Result:
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
The flash Point of given sample determined by Cleveland’s apparatus is found to be --------˚C
The fire Point of given sample determined by Cleveland’s apparatus is found to be --------˚C
Precaution:
1. The oil cup should be properly dried to ensure no moisture inside it.
2. The bulb of thermometer should dip inside the oil sample.
3. Stirring of the oil should be stopped at the time of the application of test flame.
4. Breathing over the surface of the oil should be avoided.
5. A bluish halo sometimes found around the test flame should not be confused with the flash.
Experiment No.10
Aim: To determine moisture, volatile matter, ash content and fixed carbon of a given sample
of Coal by proximate analysis
Apparatus: Silica crucible with vented lid, electric oven, Muffle furnace, spatula, desicator, pair of
tongs, weighing balance, long legged tongs, etc.
Chemicals: Powdered coal sample.
Theory: Coal is a primary, solid, fossil fuel. Coal sample has to be analyzed before using it in any
field/industry to find out its quality & suitability. Moisture, volatile matter & ash content of coal are
determined under proximate analysis. This method is simple & quick and is used primarily to
determine the suitability of coal for coking, power generation or for iron ore smelting in the
manufacture of steel.
Moisture: Moisture held within the coal itself is known as inherent moisture & is analyzed.
Moisture reduces the calorific value of coal and considerable amount of heat is wasted in
evaporating it during combustion. Moisture content should be as low as Possible.
Volatile matter: Volatile matter is usually a mixture of short & long chain hydrocarbons, aromatic
hydrocarbons and some sulfur. Volatile matter of the coal is related to the length of the flame,
smoke formation & ignition characteristics. High volatile matter coal gives long flame, high smoke
& relatively low heating values. Volatile matter content should be low but minimum 20% is
required for the ignition of coal.
Ash: Ash content of coal is the non-combustible residue left after coal is burnt. It consists of
inorganic matter like silica, alumina, iron oxide, lime, magnesia, etc. Ash reduces the heating value
of coal, reduces air supply in furnaces and also requires labour (extra cost) for its regular disposal.
Therefore ash content of coal should be as low as possible.
Fixed carbon: The fixed carbon content of the coal is the carbon found in the material which is left
after volatile materials are driven off. More the fixed carbon content, higher will be the calorific
value of coal.
Procedure:
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
B. Determination of Volatile matter: The dried sample of coal after determining moisture content
is closed with a vented lid. The closed crucible is then heated in muffle furnace maintained at 925 ±
20o C for exactly 7 minutes. The crucible is taken out from Muffle furnace carefully with the help
of long legged tongs. It is first cooled in air and then in a desiccator. When the crucible attains room
temperature it is weighed. Calculate the loss in weight.
C. Determination of Ash: Transfer about 1g (known quantity) of powdered air dried coal sample
into a previously weighed silica crucible. Place the open crucible with sample in a Muffle furnace
maintained at 725 ± 25o C for about 40 minutes or till constant weight is obtained. Coal burns in
open and the residue left is ash. Take out the crucible from Muffle furnace carefully using long
legged tongs. Cool the hot crucible first in air and then in a desiccator. Weigh the crucible and find
out the amount of unburnt residue left (ash).
A. For Moisture:
B.
1. Weight of empty crucible = W1 = ________ g.
2. Weight of crucible + Coal sample = W2 = _________ g.
3. Weight of Coal sample before heating = W2 – W1 = W3 = _________ g.
4. Weight of crucible + Sample after heating for 1 hr at 105 –110oC = W4 =_______ g.
5. Weight of Coal sample after heating = W4 – W1 = W5 = ___________ g.
6. Loss in weight of sample due to moisture = W3 – W5
OR W2 – W4 = WM = ______g.
Weight of moisture WM
% Of Moisture in coal = x 100 = x 100
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
= _____ %
= _____ %
C. For Ash:
Weight of Ash WA
% Of Ash in coal = x 100 = x 100
Weight of coal (before heating) W3
= _____ %
Results :
The coal sample contains:
1. Moisture = _______ %
2. Volatile matter = _______ %
3. Ash = _______ %
4. Fixed Carbon = _______ %
Conclusion: Quality of coal is good /Poor
Precaution:
1. Collect the homogenized sample into a clean, sealable plastic cup or glass bottle.
2. Store the sample in a refrigerator or freezer until required.
3. Ensure that the prepared sample is still homogeneous prior to weighing. If liquid separates
from the sample, re blend before use.
4. Make certain that the vents on the hoods are open; switch on electrical power to the exhaust
system.
---------------------------------
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Experiment No.11
Procedure:-
1. Place 5 ml of glacial acetic acid and 2.5 ml of 40% formaldehyde solution in a 100 ml
beaker .
2. Add 2 g of phenol to it.
3. Wrap a cloth loosely round the beaker. Add a few ml of conc. HCl in to the mixture
carefully and heat it slightly.
4. A large mass of plastic pink in colour is formed.
5. A residue is washed with water and filtered.
6. The product dried and yield is weighed.
Observations:-
Mass of the beaker (W1) = ---------g.
Mass of the beaker with phenol formaldehyde (W2) = --------g.
Therefore mass of phenol formaldehyde (W2 – W1) = --------g.
Properties:-
1. Phenol formaldehyde moulding resins have excellent heat resistance.
2. These have high dimensional stability.
3. Phenolic resins have good dielectric properties.
4. They have hard, regid and scratch resistant.
Precautions:-
1. While adding conc. HCl, it is better to stay little away from the beaker since the reaction
sometimes becomes vigorous.
2. The reaction mixture should be stirred continuously.
---------------------------------
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Experiment No.12
Apparatus required: Beaker, glass rod, funnel, filter paper and chemical balance.
Theory: Amino resins are condensation products obtained by the reaction of formaldehyde with
nitrogen bearing compounds such as aniline, amides for ex:- melamine formaldehyde, urea
formaldehyde etc. Urea formaldehyde is prepared by condensation reaction between urea and
formaldehyde in acidic or alkaline medium. The first product formed during the formation of resin
is monomethylol and dimethylol ureas. Polymerization can take place from mono or dimethylol
urea or possibly through both, with the formation of long chains.
Procedure:
1. Place about 5 ml of 40% formaldehyde solution in 100 ml beaker.
2. Add about 2.5 g of urea with constant stirring till saturated solution is obtained.
3. Add a few drops of conc. H2SO4, with constant stirring.
4. A voluminous white solid mass appears in the beaker.
5. Wash the white solid with water and dry it in the folds of filter paper.
6. Weight the yield of product
Observations:-
Mass of the beaker (W1) = ---------g.
Mass of the beaker with urea formaldehyde (W2) = --------g.
Therefore mass of urea formaldehyde (W2 – W1) = --------g.
Properties:
1. They have good electrical insulating properties.
2. They are resistant to oil, grease and weak acids.
3. They are hard, resist abrasion and scratching.
4. They have good adhesive properties.
Uses:-
1. They are used adhesive applications for the production of plywood and laminating.
2. They are used for the manufacture of cation exchange resins.
3. These also find use in the manufacture of electrical switches, plugs and insulating foams.
4. Their applications also include the treatment of textile fibers for improving their shrink and
crease resistance.
Precautions:
1. While adding concentrated H2SO4, it is better to stay little away from the beaker since the
reaction sometimes becomes vigorous.
2. The reaction mixture should be stirred continuously.
---------------------------------
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
Experiment No.13
Requirement: Fresh spinach leaf, mortar and pestle, chromatographic solvent, chromatographic
paper, chromatographic chamber, capillary tube, watch glass, scale and pencil
Theory:
In paper chromatography, the stationary phase is a special quality paper called chromatography
paper. Mobile phase is a solvent or a mixture of solvents. A solution of the mixture is spotted on a
line about 2 cm above from the bottom of the paper, called original line or base line and then
suspended in a chromatography chamber containing suitable solvent. The solvent rises up the paper
by capillary action and flows over the spot. The paper selectively retains different components
according to their differing partition in the two phases. The paper strip so developed is called
Chromatogram. The spots of the separated coloured compounds are visible at different heights from
the position of initial spot on the chromatogram. The spots of the separated colourless components
may be observed either under ultraviolet light or by the use of an appropriate spray reagent. The
distance travelled by the solvent from the original line is called solvent front. The relative
adsorption of each component of the mixture is expressed in terms of its Retardation factor (Rf)
(Retention factor or relative flow value).
Procedure:
6. Take a strip of chromatography paper having a narrow notch at one end of the strip.
7. Take a pencil and a scale and draw a horizontal line with a pencil about 2-3 cm away from
the tip of the notch.
Put
8. A drop of the pigment extract in the middle of the line with the help of a capillary tube.
9. Allow the drop to dry and repeat till four or five drops are placed on the paper.
10. Take the chromatographic chamber and pour ether acetone solvent in it.
11. Fold one end of the filter paper strip and staple it.
12. Using a thread, hang the filter paper strip in the chromatographic chamber.
13. The loading spot should remain about 1 cm above the solvent level.
14. Leave the chromatographic chamber undisturbed for some time.
15. We can observe, as the solvent moves through the paper, it spreads the different pigments of
the mixture to various distances.
16. When the solvent rises about 3/4th up the strip, remove the strip carefully and let it dry.
Observation Table:
The dried chromatographic paper strip shows ---------- distinct colour bands.
Different pigments can be identified by their colours and Rf values of different bands can be
calculated. Compare the Rf values of observed pigment ith the values given below.
MADHAV INSTITUTE OF TECHNOLOGY AND SCIENCE GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGPV, Bhopal)
β-carotene - 0.99
chlorophyll a - 0.30
chlorophyll b - 0.13
violaxanthin - .40
lutein - .68
Calculations:
Measure the distance (in cm) of each pigment band from the loading spot and also the distance
travelled by the solvent. Calculate the Rf value of the each pigment spot using the equation and
record the values in the table.
Result:
The top most orange yellow band of pigments in the separation corresponds to carotene -Rf value =
The yellowish band appearing below it indicates the xanthophylls- Rf value =
The third from above dark green band represents chlorophyll a- Rf value =
The lowermost yellowish green band is that of chlorophyll b- Rf value =
Precaution:
8. Allow the spot to dry before putting the strip in the jar.
9. Keep the strip erect. Do not let it curl.
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