Practical Manual 2023-24

MADHAV INSTITUTE OF TECHNOLOGY & SCIENCE, GWALIOR
(A Govt. Aided UGC Autonomous Institute Affiliated to RGpV, Bhopal)

NAAC Accredited with A+ + Grade
LAB MANUAL
ENGINEERING CHEMISTRY
3000002
Year 2023-24
Subject: Engineering Chemistry laboratory (Common to B.TECH. I st year-all branch)

Paper code 3000002
To provide students with practical knowledge of quantitative analysis of materials by classical and
instrumental methods for developing experimental skills in building technical competence.
Course Outcomes: On completion of this course, students will be able to
Course outcome Course outcome – Upon successful completion of the course, the student will
be able to
CO1 Develop experimental skill required for application of chemistry in engineering.
Operate different chemicals and instruments specified in course safely and

CO2
efficiently.
CO3 Analyse water sample, lubricants, fuel, alloys and ores for different properties
CO4 Function as a member of a problem solving team

List of Experiments
Subject: Engineering Chemistry laboratory (Common to B.TECH. Ist, IInd year -all branch)
Paper code 3000002
NOTE: At least 10 of the following core experiments must be performed during the session.
Expe Aim of experiment

rime
nt no.
1 Determination of Total hardness by Complexometric titration.
2 Determination of temporary and permanent hardness by Complexometric titration.
3 Determination of alkalinity of given water sample by neutralization Titration.

(a) OH & C03
(b) C03 & HCO3
4 Determination of percentage of Fe in Iron alloy solution by redox titration.
5 Determination of percentage of Cr in Chromium alloy solution by back titration.
6 Determination of Cu in Copper alloys solution by Iodometric Titration.
7 Determination of Viscosity of given oil sample by Redwood viscometer No.1

8 Determination of Flash & fire points of given oil sample by Pensky Martin close cup
Apparatus.
9 Determination of Flash & fire point of given oil sample by Cleveland's open cup
Apparatus.
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.
12 Preparation of urea formaldehyde resin by condensation polymerization.
13 Separation of the colour pigment of spinach leaf by paper chromatography.

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 or smell 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.
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) Aim of the experiment.
c) Requirement of chemicals, glassware and apparatus
d) Theory of experiment.
e) Procedure including sources of error.
f) Precautions taken to eliminate or to minimize the errors.
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 with formula used.
d) Graph sheets and other papers to be attached if required.
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.
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.
[Ca / Mg –EBT] + EDTA [Ca / Mg –EDTA] + EBT

(Wine red/unstable) (Stable colourless) (Blue)
Structure of di-sodium salt of EDTA:
Structure of EBT Indicator:

Structure of Metal EDTA complex
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:
S.no. Volume of water Burette Reading (mL) Volume of EDTA used

sample( ml) (mL)
10 ml
Calculation:
Volume of EDTA x 1000

Total Hardness =
(ppm) Volume of water sample taken
RESULT: The Total hardness of given water sample is-------------- ppm
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.
---------------------------------
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.
[Ca / Mg –EBT] + EDTA [Ca / Mg –EDTA] + EBT

(Wine red/unstable) (Stable colourless) (Blue)
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. 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:
S.no. Volume of water ) Burette Reading (mL Volume of EDTA used

sample( ml) (mL)
10 ml
Boiled 10 ml
water
Calculation:
Volume of EDTA x 1000
Total Hardness =
Volume of EDTA x1000

Permanent Hardness =
(ppm) Volume of boiled water sample taken
Temporary Hardness = Total Hardness - Permanent Hardness

(ppm)
Result: The permanent hardness and temporary hardness of given water sample is ------- ------- ppm
respectively.
Precautions:
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.
---------------------------------
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)
Structure of phenolphthalein indicator

Structure of Methyl Orange indicator
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.
Reference table:
Relation Phenomenal Condition Alkalinity (ppm) alkalinity alkalinity

between Hydroxide Carbonate Bicarbonate
P&M (OH¯ ) (CO3 )
2-
(HCO3¯ )
alkalinity
P=0 If phenolphthalein end point is zero, then --------- -------- M

alkalinity is due to only bicarbonate.
P=M If methyl orange end point is zero & only P --------- --------
there is phenolphthalein end point, then the
alkalinity is due to hydroxide alone.
P = ½M If phenolphthalein end point is exactly half ------- 2P -------

the total titration, then only carbonate
alkalinity is present.
P > ½M If phenolphthalein end point is greater than 2P – M 2( M – P ) -------

half the total titration, then alkalinity is due
to both carbonate & hydroxide.
P<½M If phenolphthalein end point is less than half ------- 2P M – 2P

the total titration, then alkalinity is due to
both carbonate & bicarbonate.
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
2
3
4
Calculations:
V1 x Normality of HCl x 50000
Phenolphthalein alkalinity (P) =
V2 x Normality of HCl x 50000

Methyl orange alkalinity (M) =
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.
---------------------------------
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.
MnO4 − + 8H+ + 5e = Mn2+ + 4H2O
Therefore, equivalent weight of KMnO4 = (Molecular weight of KMnO4)/ 5
Similarly, for the oxidation of Fe2+ Fe3+ ion
Fe 2+ – e = Fe 3+
Therefore, equivalent weight of Ferrous salt = (Molecular weight of Ferrous salt)/1
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.
MnO4 − + 8H+ + 5e Mn2+ + 4 H2O

Fe 2+ – e Fe 3+ x 5
___________________________________________
MnO4 − + 8H+ + 5 Fe2+ Mn2+ + 5 Fe3+ + 4 H2O (Ionic equation)
The actual equation is:
2 KMnO4 + 10 FeSO4 + 8 H2SO4 K2SO4 + 2MnSO4 + 5 Fe2 (SO4)3 + 8 H2O
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.
MnO4 – + 8H+ + 5e  Mn2+ + 4 H2O

(purple) (colourless)
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
S.no. Volumeof FAS Taken Burette reading Volume of KMnO4 used
Calculations: Therefore, strength of KMnO4 can be calculated as follows:
N1V1 = N2V2 N1= Normality of FAS, V1= Volume of FAS
N2 = N1V1 / V2 N2= Normality of KMnO4, V2= Volume of KMnO4

Observations Table 2:
KMnO4 vs. Fe alloy

S.no. Volume of FAS Taken Burette reading Volume of KMnO4 used
Calculations: Therefore, strength of Iron alloy can be calculated as follows:
N2V2 = N3V3 N2= Normality of KMnO4 ,V2= Volume of KMnO4
N3 = N2V2 / V3 N3= Normality of Fe alloy ,V3= Volume of Fe alloy
Strength gm/litre = Normality N3 x Equivalent weight of iron
Percentage of iron = 3 gm/litre of iron alloy contains =……….gm of iron

100 gm/litre of iron alloy contains =……….% of iron
Result: The percentage of iron in a given iron alloy solution is ………%
Precaution:
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.
-------------------------------
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+
Cr2O72- + 6Fe2+ + 14H+ 2Cr3+ + 6Fe3+ +7H2O

(alloy) (FAS) (green)
The remaining FAS is back titrated with KMno4 and oxidized to Fe3+ ion and KMno4 reduced to
colourless manganous ions.
5Fe2+ + Mno4- + 8H+ Mn2+ + 5Fe3+ + 4H2O

Chemicals: Chromium alloy solution , N/40 FAS Solution, N/40 KMno4 Solution.
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.
Observation Table:
S.No. Volume of Alloy Burette Reading Volume of KMno4 Volume of FAS

Used used
20-B.R.
Calculation:-
N1 V1 = N2V2
N2=N1V1/V2
N1 = Normality of FAS solution

V1 = Volume of FAS used with alloy (50-B.R.)
N2 = Normality of Alloy solution
V2 = Volume of Alloy solution
Strength gm/liter = N2 x Equivalent weight of Chromium
3gm of Chromium alloy contains = ---------gm of Chromium
100 of Chromium alloy contains = --------% of Chromium
Result:-
The % of Chromium present in a given Chromium alloy Solution is ---------%.
Precautions:
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.
------------------------------
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.

Chemicals: Sodium thio sulphate (Hypo) solution, Starch Indicator, KI Solution, Copper alloy
Solution .
Theory: Copper in copper alloy is determined by iodometric method. When KI is added to a solution of
copper alloy white cuprous iodide (Cu2I2) is precipitated and an equivalent amount of chlorine of iodine
is liberated. This free iodine is titrated against slandered solution of Hypo, using starch as indicator. As
soon as all the liberated iodine has been reduced to iodine (NaI), the blue colour of iodostarch complex
will disappear and the colour of precipitated in the conical flask will be white due to formation of
cuprous iodine. This indicate end point.
2CuSO4 + 4KI 2CuI + 2K2SO4 +I2

White ppt.
2NaS2O3 +I2 Na2 S4O6 + NaI

Sod. Tetrathionate
Hence 2CuSO4.5H2O = I2 = 2Na2S2O3
Procedure:-
1. Fill a clean burette with Na2S2O3 solution
2. Take 10 ml of Copper alloy solution in a conical flask.
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
N1 = Normality of Hypo solution

V1 = Volume of Hypo solution
N2 = Normality of Alloy solution
V2 = Volume of Alloy solution
Strength in gm/L = N2 x Equivalent weight of Copper
Percentage of copper =
3 gm/litre of copper alloy contains =……….gm of copper
100 gm/litre of copper alloy contains =……….% of copper
Result: The percentage of Copper in a given Copper alloy solution is-------------%
Precautions:
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.
Viscometers Diameter of orifis Length of the jet

Redwood viscometer No.1 1.62 mm 10 mm
Redwood viscometer No.2 3.8mm 50 mm
Redwood viscometer No.1 is commonly used for light or thin oil (kerosene, mustered oil etc.)
Redwood viscometer No.2 for highly viscous oils (fuel oil, mobile oil, glycerol etc.)
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.
Observation table:
S. no. Time taken for 50 ml of oil Time taken for 50 ml of

in redwood seconds oil in redwood seconds
At room temperature At 60˚C
Result: The viscosity of given lubricating oil at room temp…………….

The viscosity of given lubricating oil at 60˚C …………….
Precautions:
1. Redwood viscometer should be clean.
2. Stopwatch should be started at accurate time i.e. at which the oil starts flow.
3. Stopwatch should be stopped at the time when oil finished.

4. kohlrausch flask should be placed in such a way that the oil jet touches the inside layer of the
flask and does not cause foaming.
-------------------------------
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, 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
0
C 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
Precaution:
1. The oil cp 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.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 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:
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:
A. Determination of Inherent Moisture: Transfer about 1g (known quantity) of powdered air dried
coal sample into a previously weighed silica crucible. Place the open crucible with sample in an electric
oven and heat it at about 105 –110oC for an hour. Take out the crucible after one hour from the oven and
cool it in a desiccators (containing moisture absorbing anhydrous calcium chloride). Then weigh the
crucible with sample and repeat the process of heating, cooling & weighing till constant weight is
obtained. Calculate the loss in weight.
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).
D. Determination of Fixed Carbon: The percentage of fixed carbon is determined

indirectly by substracting the sum total percentages of moisture, volatile matter & ash from 100.
Observations and Calculations: (All weights are in grams, g)
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
Weight of coal (before heating) W3
= _____ %
B. For Volatile matter:
1. Weight of empty crucible = W1 (W1 from part A) = __________ g.

2. Weight of crucible + moisture free coal sample = W2 (W4 from part A) = _______ g.
3. Weight of moisture free sample (before heating) = W2 – W1 = W3 = _________g.
4. Weight of crucible + Sample after heating for 7 mins. at 925 ± 20o C = W4 =_____g.
5. Weight of Sample after heating = W4 – W1 = W5 = ___________ g.

6. Loss in weight of sample due to volatile matter = W3 – W5 = WVM = ________ g.
Weight of volatile matter WVM

% Of Volatile matter in coal = x 100 = x 100
= _____ %
C. For Ash:
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 40 mins. at 725 ± 25o C = W4 =______g.
5. Weight of Ash formed = W4 – W1 = WA = ___________ g.
Weight of Ash WA
% Of Ash in coal = x 100 = x 100
= _____ %
D. For Fixed carbon (FC):
% Of Fixed Carbon = 100 – (% Moisture + % Volatile matter + % Ash)
= 100 – ( ________ ) = 100 – ______ = ______ %
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.
---------------------------------
Experiment No.11
Aim:- To prepare phenol formaldehyde resin by condensation polymerization.

Apparatus:- Beaker, glass rod, funnel, filter paper, and chemical balance.
Chemicals:- Phenol, formaldehyde, conc. HCl, glacial acetic acid, distilled water.
Theory:- Phenolic resins are condensation polymerization of phenolic derivatives (like phenol,
resorcinol) with aldehyde (like formaldehyde, furfural). Most important member of this
class is bakelite or phenol formaldehyde resin. Phenol formaldehyde is prepared by condensing phenol
with formaldehyde in presence of acidic or alkaline catalyst. The initial reaction result in the formation
of o- and p-hydroxy methyl phenol, which react to form linear polymer navalac. During moulding
hexamethyline tetramine [ (CH2)6N4] is added which convert the fusible novalac in to hard infusible
and insoluble solid of cross – linked structure known as resol .
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.
Result: - The yield of phenol formaldehyde is = --------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.
---------------------------------
Experiment No.12
Aim: To prepare urea formaldehyde resin by condensation polymerization.
Apparatus required: Beaker, glass rod, funnel, filter paper and chemical balance.
Chemicals: Urea, formaldehyde sol., conc. H2SO4, distilled water.
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.
Urea formaldehyde resin.
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.
Result:- The yield of urea formaldehyde = -------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.
---------------------------------
Experiment No.13
Aim: To separate the colour pigment of spinach leaf by paper chromatography.
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).
Distance travelled by the sample component from origin

Rf =
Distance travelled by the solvent from origin
Procedure:
1. Take a few freshly plucked green spinach leaves.

2. Cut the spinach leaves into small pieces and let them fall into the mortar.
3. Take a measuring cylinder that contains 5ml of acetone and pour it into the mortar.
4. Grind the spinach leaves using the mortar and pestle.
5. Place the extract into a watch glass using a spatula.
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.
S.no. Pigment Distance travelled in cm Rf value calculated

colour
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.
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.
Distance travelled by the sample component

Rf value =
Distance travelled by the solvent
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:
1. Spinach leaves should be fresh and green.

2. The loading spot should be 2-3 cm away from the tip of the notch.
3. While hanging the strips in the chromatography chamber, the loading spot should remain above
the solvent level. Do not allow the spot to dip in the solvent.
4. Use good quality pencil for drawing the reference line so that the mark does not dissolve in the
solvent in which the chromatography is carried out.
5. Always use a fine capillary tube.
6. Keep the jar undisturbed and covered during the experiment.
7. The spot should be small and rich in mixture.
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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MADHAV INSTITUTE OF TECHNOLOGY & SCIENCE, GWALIOR

(A Govt. Aided UGC Autonomous Institute Affiliated to RGpV, Bhopal)

Subject: Engineering Chemistry laboratory (Common to B.TECH. I st year-all branch)

Course Outcomes: On completion of this course, students will be able to

CO1 Develop experimental skill required for application of chemistry in engineering.

Operate different chemicals and instruments specified in course safely and

CO4 Function as a member of a problem solving team

Expe Aim of experiment

1 Determination of Total hardness by Complexometric titration.

2 Determination of temporary and permanent hardness by Complexometric titration.

3 Determination of alkalinity of given water sample by neutralization Titration.

5 Determination of percentage of Cr in Chromium alloy solution by back titration.

6 Determination of Cu in Copper alloys solution by Iodometric Titration.

7 Determination of Viscosity of given oil sample by Redwood viscometer No.1

12 Preparation of urea formaldehyde resin by condensation polymerization.

13 Separation of the colour pigment of spinach leaf by paper chromatography.

GENERAL PRECAUTIONS TO BE TAKEN IN THE LABARATORY

INSTRUCTIONS FOR RECORD WRITING

1. Write on the right hand page the following order:

[Ca / Mg –EBT] + EDTA [Ca / Mg –EDTA] + EBT

Structure of di-sodium salt of EDTA:

Structure of EBT Indicator:

Structure of Metal EDTA complex

S.no. Volume of water Burette Reading (mL) Volume of EDTA used

Volume of EDTA x 1000

(ppm) Volume of water sample taken

RESULT: The Total hardness of given water sample is-------------- ppm

[Ca / Mg –EBT] + EDTA [Ca / Mg –EDTA] + EBT

S.no. Volume of water ) Burette Reading (mL Volume of EDTA used

Volume of EDTA x1000

Temporary Hardness = Total Hardness - Permanent Hardness

Structure of phenolphthalein indicator

Structure of Methyl Orange indicator

Relation Phenomenal Condition Alkalinity (ppm) alkalinity alkalinity

P=0 If phenolphthalein end point is zero, then --------- -------- M

P = ½M If phenolphthalein end point is exactly half ------- 2P -------

P > ½M If phenolphthalein end point is greater than 2P – M 2( M – P ) -------

P<½M If phenolphthalein end point is less than half ------- 2P M – 2P

V2 x Normality of HCl x 50000

The same amount of indicator should be used in all titrations.

MnO4 − + 8H+ + 5e = Mn2+ + 4H2O

Therefore, equivalent weight of KMnO4 = (Molecular weight of KMnO4)/ 5

Similarly, for the oxidation of Fe2+ Fe3+ ion

Therefore, equivalent weight of Ferrous salt = (Molecular weight of Ferrous salt)/1

MnO4 − + 8H+ + 5e Mn2+ + 4 H2O

The actual equation is:

2 KMnO4 + 10 FeSO4 + 8 H2SO4 K2SO4 + 2MnSO4 + 5 Fe2 (SO4)3 + 8 H2O

MnO4 – + 8H+ + 5e  Mn2+ + 4 H2O

S.no. Volumeof FAS Taken Burette reading Volume of KMnO4 used

Calculations: Therefore, strength of KMnO4 can be calculated as follows:

N1V1 = N2V2 N1= Normality of FAS, V1= Volume of FAS

N2 = N1V1 / V2 N2= Normality of KMnO4, V2= Volume of KMnO4

KMnO4 vs. Fe alloy

Calculations: Therefore, strength of Iron alloy can be calculated as follows:

N2V2 = N3V3 N2= Normality of KMnO4 ,V2= Volume of KMnO4

N3 = N2V2 / V3 N3= Normality of Fe alloy ,V3= Volume of Fe alloy

Strength gm/litre = Normality N3 x Equivalent weight of iron

Percentage of iron = 3 gm/litre of iron alloy contains =……….gm of iron

Result: The percentage of iron in a given iron alloy solution is ………%

Cr2O72- + 6Fe2+ + 14H+ 2Cr3+ + 6Fe3+ +7H2O

5Fe2+ + Mno4- + 8H+ Mn2+ + 5Fe3+ + 4H2O

Apparatus: Pipette, Burette, conical flask, beaker, funnel.

S.No. Volume of Alloy Burette Reading Volume of KMno4 Volume of FAS

= 100 – ( ) = 100 – = %