Chemistry Laboratory Manual 2023-24

LABORATORY MANUAL
ENGINEERING CHEMISTRY for CSE

Stream (BCHES102/202)
FOR THE ODD & EVEN SEMESTERS OF 1ST YEAR STUDENTS
Name
USN
Branch & Section
Batch
ATRIA INSTITUTE OF TECHNOLOGY

Anandanagar, Bengaluru – 560 024
Department of Chemistry (BSE&H) Atria Institute of Technology
PRACTICAL MODULE
Chemistry for CSE Stream (BCHES102 / 202)
A – Demonstration (any two) offline/virtual:

A1. Chemical Structure drawing using software: Chem Draw or ACD/ChemSketch
A2. Estimate the amount of copper in e-waste by optical sensors (colorimetry)
A3: Synthesis of Iron-oxide Nanoparticles
A4. Electrolysis of water
B – Exercise (compulsorily any three):
B1. Conductometric estimation of acid mixture
B2. Potentiometric estimation of FAS using K2Cr2O7
B3. Determination of pKa of vinegar using pH sensor (Glass electrode)
B4. Determination of rate of corrosion of mild steel by weight loss method
B5: Estimation of total hardness of water by EDTA method
C – Structured Enquiry (compulsorily any three):
C1. Estimation of Copper present in electroplating effluent by optical sensor (colorimetry)
C2. Determination of Viscosity coefficient of lubricant (Ostwald’s viscometer)
C3. Estimation of Iron in TMT bar by diphenyl amine method
C4. Estimation of Sodium present in soil/effluent sample using flame photometer
C5. Determination of Chemical Oxygen Demand (COD)of industrial waste water sample
D – Open Ended Experiments (any two):
D1: Evaluation of acid content in beverages by using pH sensors and simulation.
D2. Construction of photovoltaic cell.
D3. Design an experiment to identify the presence of proteins in given sample.
D4. Searching suitable PDB file and target for molecular docking.
2
General Instructions
To be a better analyst, understand the theory of the experiments you conduct.

Keep your working table tidy/clean and organized.
Keep the apparatus scrupulously clean.
keep the reagents in their proper places after use. Do not later their position.
Do not contaminated the reagents.
Keep gas taps and water taps close whenever not in use.
Do not throw any wastepaper and litmus paper into the sink and dispose them into dust
bin.
Do not pour concentrated acids into the sink. If they are to be poured, flush them with
water (liberally).
Record your observations as and when you performed the test (and not after completion).
3
Instructions for Volumetric Analysis
BURETTE
Wash burette with tap water and then rinse with distilled water.
Rinse burette with a small volume of solution to be taken in burette and discard the
solution into sink.
Fill the burette with the solution using a small funnel which is already washed with
tap water, rinsed with distilled water and then with the solution.
Remove the funnel from the burette before starting the titration.
Record the initial and final readings properly keeping the burette straight to your eye
level.
During the addition of the solution from burette, the conical flask mut be constantly
swirled with one hand while the other hand controls the stop cock of the burette.
PIPETTE
Wash pipette with tap water and then rinse with distilled water.
Rinse pipette with a small volume of solution to be taken in the pipette and discard
the same into sink.
Do not blow out the last drops of the liquid from the pipette.
CONICAL FLASK
Wash the conical flask with the tap water and then rinse with the distilled water.
Do not try to drain out the water particles from the conical flask.
During the titration, place the conical flask on a glazed white tile below the burette.
4
Experiment - 1
A3. Synthesis of Iron-oxide Nanoparticles
Aim : To synthesize iron oxide nanoparticles using co-precipitation method.
Chemicals required
Iron (II) chloride (FeCl2.4H2O), Iron (III) chloride (FeCl3, anhydrous), sodium hydroxide (NaOH)
and deionized water.
Preparation
1) Take 0.7954 g of iron (II) chloride and 1.2974 g of iron (III) chloride and dissolve in distilled
water. The mole ratio of iron (II) chloride and iron (III) chloride needs to be fixed at 1:2
throughout the experiment.
2) The solution is then mixed for 30 minutes by using hot plate with magnetic stirrer.
3) After that, the mixed solution is separated by using centrifuge at 4000 rpm for 15 minutes.
4) The separated precipitate is dried in the oven at temperature of 100 °C for 24 hours.
5) Finally, the resulted dark brown precipitate sample is collected and crushed into fine powder by
using a pestle and mortar.
6) The chemical balanced equation for the reaction FeCl 2.4H2O and FeCl3 is shown below, where
Fe2O3 is the final product and water is the by-product;
𝐹𝑒2+ + 2𝐹𝑒3+ + 8𝑂𝐻− 𝐹𝑒3𝑂4 + 4𝐻2𝑂

𝐹𝑒3𝑂4 + 0.25 𝑂2 + 4.5𝐻2𝑂 3(𝑂𝐻)3
2(𝑂𝐻)3 𝐹𝑒2𝑂3 + 3𝐻2𝑂
Result :
Fe2O3 nanoparticles have been successfully prepared using co-precipitation method
1
Experiment - 2
B1. Conductometric estimation of acid mixture
Aim : Estimation of acid mixture conductometrically using standard NaOH solution.
Principle
The principle underlying conductometric titrations is the substitution of ions of one mobility by ions
of other mobility. Therefore, the conductance of a solution depends on the number & mobility of
ions. The equivalence point is determined graphically by plotting conductance against titre values.
Conductometric titration may be applied for the determination of acid mixture. In this titration, on
adding a strong base to a mixture of a strong acid and a weak acid, the conductance falls till a strong
acid is neutralized completely due to removal of H+ ions. The weak acid remains undissociated in the
presence of strong acid. Once the strong acid is completely neutralized, the weak acid begins to
dissociate and gets neutralized. This results in increase of conductance of solution. When the
neutralization of second acid is complete, there will be steep increase in conductance due to the ions
furnished by strong base.
Procedure
1) Pipette out 25 cm3 of acid mixture in a 250 ml beaker.

2) Immerse the conductivity cell in the given solution and connect it to conductivity meter. Stir the
solution and measure the initial conductance of the solution.
3) Add std. NaOH from the burette in the increments of 0.5 cm3 after each addition stir the solution
and note down the conductance.
4) Continue the titration till decreasing trend changes to increasing trend.
5) Plot the graph of conductance on Y-axis and volume of NaOH on X-axis to get two straight lines.
The point of intersection of two straight lines gives the equivalence point.
The equivalence point corresponds to volume of NaOH required to neutralize HCl.
6) By knowing the normality & volume of NaOH calculate the normality & amount of HCl &
CH3COOH.
2
OBSERVATION & CALCULATION
Burette: 0.5 N NaOH solution

Electrode: Conductivity cell (Platinum electrode)
Beaker: 25cm3 of acid mixture + 1 test tube distilled water
Volume of NaOH Conductance

(cm3) (ohm-1cm-1)
0.0
0.5
1.0
1.5
2.0
Conductance
2.5
3.0
3.5
4.0
4.5 Volume of NaOH
5.0
5.5 where,
6.0 V1 = Volume of NaOH required to neutralize HCl
6.5 (V2 - V1 ) = Volume of NaOH required to

neutralize acetic acid
7.0
7.5
8.0
8.5
9.0
9.5
3
(NV) HCl = (NV) NaOH
(𝐍 𝐱 𝐕) 𝐍𝐚𝐎𝐇
 NHCl =
𝐕𝐇𝐂𝐥
. ( )
=
= …………. N
Weight of HCl in one litre of the solution = NHCl Ⅹ Eq.wt. of HCl (36.5)
=……………….g/dm3
(𝐍 𝐱 𝐕) 𝐍𝐚𝐎𝐇
 NCH3COOH =
𝐕𝐚𝐜𝐞𝐭𝐢𝐜 𝐚𝐜𝐢𝐝
. ( )
= =
= …………….. N
Weight of CH3COOH/ litre of solution = NCH3COOH x Eq. wt. of CH3COOH (60)
= …………… g/dm3
Result :
(i) Normality of HCl = NHCl =………………….. N
(ii) Normality of CH3COOH = NCH3COOH …………….. N
(iii) Amount of HCl per litre of solution = …………….. g/litre
(iv) Amount of CH3COOH per litre of solution = ………….. g/litre
4
Experiment - 3
B2. Potentiometric estimation of FAS using K2Cr2O7
Aim
To estimate the amount of ferrous ammonium sulphate (FAS) using standard potassium dichromate
potentiometrically.
Principle
A potentiometric titration involves the measurement of change in potential with a suitable electrode
which responds to the change in concentration during the titration. The electrode which responds to
the change in concentration of ion in the solution is called indicator electrode. The indicator electrode
is combined with reference electrode (whose potential does not change during the titration) to form
a cell and E.M.F. of the cell changes gradually till the end point and changes rapidly at very close to
the end point and again the change is gradual after the end point.
A plot the first derivative curve, in which (∆E/∆V) is plotted against V, the peak of the curve gives
the end point of the titration.
The potentiometric titration of FAS (Mohr’s salt) solution with K2Cr2O7 in the presence of H2SO4 is
a redox titration.
3Fe2+ + Cr6+ → 3Fe3+ + Cr3+ [Acidic medium]
The presence of oxidized and reduced form of the same substance in a solution gives rise to the
formation of an oxidation-reduction electrode, developing an electrode potential, which can be picked
up by dipping a Platinum wire. Thus, when the titration is commenced, both Fe 2+and Fe3+ ions are
present in the solution, developing an electrode potential which is picked up by a Pt wire. Thus
(Pt/Fe3, Fe2+) is the indicator electrode, whose electrode potential is given by,
E= E0 + 2.303 RT log (Fe3+)

nF (Fe2+)
During the titration (Fe3+) goes on increasing and (Fe2+) goes on decreasing as K2Cr2O7 solution is
added continuously, gradually changing the potential. Near the end point the ration (Fe 3+ / Fe2+)
increases rapidly as (Fe2+) becomes very small and tending to zero at the end point. Thus, the E.M.F
increases rapidly at very close to the end point. When Fe 2+ is completely converted into Fe3+ by
K2Cr2O7, the electrode, (Pt/Fe3+, Fe2+) ceases to exit. But the presence of slight excess of K 2Cr2O7,
brings in existence of (Pt/Cr6+, Cr3+) electrode. Thus, after the end point, it is the electrode potential
of the (Pt/Cr6+, Cr3+) electrode, which is going to change. Because of both the factors i.e., increase in
5
the value of (Fe3+/ Fe2+) and change of electrode from (Pt/Fe3+, Fe2+) to (Pt/Cr6+, Cr3+) there is a large
change in potential at the end point.
Procedure
1) Pipette out 25 cm3 of ferrous ammonium sulphate into a beaker.

2) Add two test tubes of dilute sulphuric acid. Immerse calomel and platinum electrode assembly
into it.
3) Stir the solution and measure the initial potential of the solution.
4) Add std. potassium dichromate from the burette in the increments of 0.5 cm3, after each
addition stir the solution and note down the potential.
5) Continue the procedure till the potential shows the tendency to increase rapidly.
6) Plot a graph of ∆E/∆V against volume of potassium dichromate and determine the
equivalence point from the graph. Calculate the normality and weight of ferrous ammonium
sulphate in the given solution.
OBSERVATION AND CALCULATIONS
Burette: 0.5 N K2Cr2O7 solution

Electrodes: Platinum electrode and Calomel electrode
Beaker: 25 cm3 of FAS solution + 2 test tubes of dilute H2SO4
Volume of E (mv) ∆V ∆E ∆𝐄
K2Cr2O7 (cm3) ∆𝐕
0.0 ---------- -------- ----------

0.5 0.5
1.0 0.5
1.5 0.5
2.0 0.5
2.5 0.5
3.0 0.5
3.5 0.5
4.0 0.5
4.5 0.5
5.0 0.5
6
5.5 0.5
6.0 0.5
6.5 0.5
7.0 0.5
7.5 0.5
8.0 0.5
8.5 0.5
9.0 0.5
∆𝐄
∆𝐕
Equivalence point (X)
Volume of K2Cr2O7
From the graph, the volume of K2Cr2O7 solution = VK2Cr2O7 =……….
N1V1= N2V2
(N x V)FAS = (N x V) potassium dichromate
(𝐍 𝐱 𝐕) 𝑲𝟐𝑪𝒓𝟐 𝑶𝟕
NFAS =
𝐕𝐅𝐀𝐒
𝟎.𝟓 𝐱 𝐕𝑲𝟐𝑪𝒓𝟐 𝑶𝟕
NFAS =
𝟐𝟓
NFAS = …………….N
Therefore, weight of FAS in a liter of solution = NFAS x Eq.wt. of FAS (392)
= NFAS x 392
=
=……………..g/ltr.
7
Result
1. Normality of the given FAS solution = NFAS = ………….. N

2. Weight of FAS in one litre of solution = ………………….. g/litre
Digital Potentiometer
8
Experiment - 4
B3. Determination of pKa of vinegar using pH sensor (Glass electrode)
Aim : To determine the pKa value of given vinegar using pH sensor (glass electrode)
Principle
Weak acids like acetic (CH3COOH), formic acid (HCOOH) etc., undergoes partial
dissociation and an equilibrium exists between ionized and unionized molecules of weak acid
hence dissociation constants Ka can be defined for weak acid. Strong acids like hydrochloric
acid (HCl) ionize completely in aqueous solution. The dissociation constant of weak (HA) like
acetic acid can be written as.
CH3COOH + H2O → CH3COO- + H3O+
[ ][ ]
Ka =
[ ]
Therefore pKa = -log Ka
Higher the value of pKa, lower is the Ka value of acid and therefore weaker is the acid. pKa
value of weak acid can be determined by the change in pH.
In the titration of acid with base, the pH of the solution gradually increases, and equivalence
point is indicated by sharp increases in pH (Fig.1). The equivalence point is determined by
plotting a graph of volume of base against ∆pH/∆V
During the titration of weak acid with base, salt of the weak acid is formed. For such an
equilibrium, according to Henderson-Hasselbalch equation.
pH= pKa + log [salt] / [acid]
At half equivalence point 50% of acid is converted into its salt and therefore
[acid] = [salt]
then, pH = pKa
therefore pH, at half equivalence point gives the pKa, value of vinegar .
Procedure
1) Pipette out 25cm3 of the given acid into a beaker and add one test tube of distilled water.
2) Immerse the glass electrode and calomel electrode assembly into it. Connect the electrode to pH
meter.
1
3) Fill the burette with sodium hydroxide. Now add sodium hydroxide from the burette in
increments of 0.5cm3 and measure pH.
4) Continue the addition of sodium hydroxide till there is slight increases in pH on the addition base.
5) Plot a graph of ∆pH/∆V against volume of sodium hydroxide added (graph-1). Determine the
equivalence point.
6) Plot another graph of pH against volume of sodium hydroxide and determine the pK a value of
weak acid from the graph as shown in graph1 and graph 2.

Burette: Sodium hydroxide solution
Electrodes: Glass electrode and Calomel electrode
Beaker: 25 cm3 of vinegar + 1 test tube of distilled water.
Volume of pH ∆V ∆pH ∆𝐩𝐇

NaOH cm3 ∆𝐕
0.0 NA NA NA
0.5 0.5
1.0 0.5
1.5 0.5
2.0 0.5
2.5 0.5
3.0 0.5
3.5 0.5
4.0 0.5
4.5 0.5
5.0 0.5
5.5 0.5
6.0 0.5
6.5 0.5
7.0 0.5
7.5 0.5
8.0 0.5
7.5 0.5
8.0 0.5
2
According to Henderson-Hasselbalch equation.

[𝐬𝐚𝐥𝐭]
pH= pKa + log
[𝐚𝐜𝐢𝐝]
At half equivalence point 50% of acid is converted into its salt and therefore
[acid] = [salt]
then, pH = pKa
∆𝐩𝐇 pKa Half equivalence

∆𝐕 point (Veq /2)
Equivalence point (Veq)
Volume of NaOH
From the graph (2) full equivalence point is Vequivalence point =………………ml
Half equivalence point is = =…………………ml
Therefore, from graph (1) at half equivalence, pH = pKa =………..
Result :
The pKa value of the given vinegar from the graph = …………..
Digital pH meter
3
Experiment - 5
B5. Estimation of total hardness of water by EDTA method
Aim :To determine the total hardness of the given sample of water using disodium salt of EDTA
Principle:
Hard water does not give lather easily with soap, as the hardness causing ions react with soap to from
insoluble soap. Hardness of water is due to presence of dissolved salts of calcium, magnesium and
other metal ions. Temporary hardness is due to bicarbonates of calcium and magnesium, which can
be removed by boiling the water. On boiling, bi carbonates are converted into insoluble carbonates
of calcium and magnesium. Permanent hardness is due to the presence of chlorides and sulphates of
calcium, magnesium and other metals, which is removed only by chemical treatment. The sum of
temporary hardness and permanent hardness is known as total hardness. The hardness is expressed
in parts per million (ppm) equivalent of calcium carbonate or mg/litre.
Hardness of water is determined by titrating a known volume of hard water sample with Na2EDTA,
using Eriochrome Black-T (EBT) as indicator, in presence of ammonium hydroxide-ammonium
chloride buffer (pH=10). Ethylene diamine tetra acetic acid (EDTA) or its disodium salt (Na 2EDTA)
is a strong complexing agent has the following structure.
Structure of EDTA
Structure of Na2EDTA
The ionization of EDTA in solution is represented as
H4Y → H2Y2- +2 H+
The anion formed in the above ionization forms complexes with metal ions M 2+ which can be given
as,
M2+ + H2Y2-→ MY2- + 2H+
When few drops of the indicator EBT is added, metal ions (Ca 2+, Mg2+) of hard water forms a wine
red coloured complex with the indicator.
M2+ + EBT → M-EBT complex (wine red)
When the solution is titrated Na2EDTA reacts, preferentially with free metal ions (Ca2+, Mg2+)
present in the solution. Near the end point, when the free metal ions are exhausted in the solution,
1
further addition of Na2EDTA dissociates the M-EBT complex, consumes the metal ions and release
free indicator, which is blue in color. Therefore, the color change is wine red to clear blue.
The indicator, EBT shows the colour change at pH range 9-11 therefore the pH of the solution is
maintained around 10 using (NH4OH + NH4Cl) buffer. EDTA being sparingly soluble in water,
generally its disodium salts (Na2EDTA) is used which readily dissolves in water. A standard solution
of Na2EDTA is prepared by dissolving a known weight of Na2EDTA in distilled water and making
up to 250ml.
Molecular weight of disodium salt of Na2EDTA = 372.24
. Ⅹ
Therefore, Molarity of Na2EDTA solution =
. . ( . )
Procedure:
(a) Preparation of standard solution of Na2EDTA :
Weigh accurately given Na2EDTA crystals and transfer it into a 250 cm3 standard volumetric flask.
Add 5 cm3 of ammonia and add ion-exchange ware to dissolve the crystals. Make up the solution to
250cm3 and mix well for uniform concentration.
(b) Determination of total hardness of water:
Pipette out 25cm3 of given hard water sample into a clean conical flask. Add 5cm3 of buffer (NH4OH
+ NH4Cl) of pH=10 and 2-4 drops of EBT indicator. Titrate this solution against standard Na 2EDTA
solution taken in a burette, until the colour of the solution changes from wine to clear blue. Repeat
the titration for concordant values.
OBSERVATION & CALCULATIONS

I. Preparation of standard Na2EDTA solution:
Weight of weighting bottle + Na2EDTA = W1=…………. g
Weight of empty weighing bottle = W2 =………………. g
Therefore, weight of Na2EDTA = (W1-W2) = W3…………… g
.
Therefore, molarity of Na2EDTA = M Na2EDTA =
. . ( . )
=
.
= ………..… M
2
II. Determination of total hardness of water:

Burette: Std. Na2EDTA solution.
Conical flask: 25cm3 hard water sample + 5 cm3 buffer solution (NH4OH+NH4Cl) of pH=10
Indicator: Eriochrome Black -T (EBT)
End point: Wine Red to clear Blue
Burette level I II III
Final burette reading
Initial burette reading
Volume of Na2EDTA (cm3)

consumed
Volume of Na2EDTA consumed = V Na2EDTA =………….cm3

Since M1V1= M2V2
(M x V) Na2EDTA = (M x V) Hard water
Therefore, M hard water = (M x V) Na2EDTA
V Hard water
= (M x V) Na2EDTA
25
M Hardwater =……………M
Therefore, Wt. of CaCO3/ litre of solution = W4 = M hard water x Mol. Wt. of CaCO3 (100)
=……….. g/dm 3
Therefore, W4 =…………. g/dm3
Total hardness of water in ppm = W4 x 106
103
= …………… ppm of CaCO 3
Result:
Total Hardness of the given sample of hard water = …………… ppm of CaCO 3.
3
Burette (Na2EDTA solution)
Experiment - 6
C1. Estimation of copper present in electroplating effluent by optical
sensor (Colorimetry)
Copper electroplating requires baths with high metal concentration, as far as 100 g/L. The
monitoring is mandatory in terms of good results of the process and safety of the wastewater
products. A colorimetric method is chosen to detect copper concentration, effective for bothhigh and
low metal amounts.
Aim : To estimate the amount of copper present in electroplating effluent by optical sensor
(colorimetric method)
Principle
Colorimetric analysis is based on measurement of quantity of light absorbed by a colored solution.
Beer-Lambert’s law forms the basis of this experiment. When a monochromatic light of intensity Io
is incident on a transparent medium, a part Ia is absorbed, a part Ir is reflected and remaining part It
is transmitted.
Therefore, Io=Ia + Ir+ It
For glass-air Ir is negligible, therefore Io= Ia+It
The ratio It/Io=T is called transmittance, log (1/T) = log (Io/It) = A, called absorbance or optical
density.
The relation between absorbance A, concentration c (in moles per liter) and path length l (in cm) is
given by Beer’s-Lambert’s law
A = Log (Io/It) = €cl
where I0= intensity of the incident light, It= Intensity of the transmitted light
c= concentration of colored solution, l= thickness of the colored medium,
€= molar absorption coefficient
So, the same result can be obtained by plotting log T against concentration also.
Cupric ions (Cu2+) react with ammonia to give a deep blue a deep blue colour due to the formation
of cuprammonium complex ion.
Cu2+ + 4NH3 → [Cu (NH3)4]2+ (Deep blue)
1
A series of standard solution containing cupric ions are treated with ammonia and the absorbance of
each of these solutions is measured at 620 nm (λ max) at which solution shows maximum absorbance.
A calibration curve is obtained by plotting concentration against absorbance or log T. The given
unknown solution is also treated with ammonia in the same way as the standard and its absorbance
is measured. Its concentration is determined from the calibration curve.
Procedure
Pipette out 2,4,6,8 and 10 cm 3 of the given copper sulphate solution (containing 8g of copper per
litre) into standard volumetric flasks add 5 cm3 of ammonia solution into each of them and make up
to the mark with distilled water and shake well.
Select a filter (620 nm) in the colorimeter and adjust the initial readings to zero absorbance with
blank solution (distilled water +ammonia) using a glass cuvette. Fill the glass cuvette with the
standard of lowest concentration and measure the absorbance. Repeat for other standard solutions
also. Plot absorbance (Y-axis) against volume (X-axis) of copper sulphate solution taken.
For the given unknown add 5 cm3 of ammonia and make up to the mark with distilled water. Measure
the absorbance using the colorimeter at the same wavelength as said above. From the graph,
determine the concentration of the unknown solution.

Wavelength of monochromatic light used for blue colour = λ max = 620 nm
Flask No. Absorbance

Volume of copper sulphate (cm3)
(Optical density)
1 2 cm3+5 ml.NH3 + H2O
2 4 cm3+5 ml.NH3 + H2O
3 6 cm3+5 ml.NH3 + H2O
4 8 cm3+5 ml.NH3 + H2O
5 10 cm3+5 ml.NH3 + H2O
Test Solution
6 (copper present in electroplating effluent
solution+ 5 ml.NH3 + H2O)
7 Blank (5 ml.NH3 + H2O)
2
Digital Colorimeter
Model graph :
249.54 g of CuSO4 contains 63.54 g of Cu
.
Therefore given 8 g of CuSO4.5H2O solution contains = 2.037 g of Cu
.
1000 cm3 of stock solution 2.037 g of copper

.
Therefore, amount of copper in unknown solution (Vtest from graph) =
= ……….g of Cu
=………. Ⅹ 10 3 mg of Cu
Result
1. The volume of copper in electroplating effluent solution from the graph =……….….. mL
2. Weight of copper (II) present in electroplating effluent =………….. mg/litre
3
Experiment - 7
C2. Determination of Viscosity coefficient of lubricant (Ostwald’s
viscometer)
Aim : To determine the viscosity co-efficient of a given lubricant using Ostwald’s Viscometer.
Principle
Viscosity is a property of liquid, defined as the resistance offered towards the flow of a layer of liquid
over the other successive layer. Viscosity arises due to internal friction between moving layers of
molecules. A liquid flowing through a cylinder tube of uniform diameter is expected to move in the
form of molecular layers. A layer close to the surface is almost stationary while layer at the axis of
tube moves faster than any other intermediate layer. The co-efficient of viscosity (Ƞ ) is defined as
tangential force per unit area required to maintain unit velocity gradient between any two successive
layers of a liquid situated unit distance apart. The viscosity co-efficient of liquid is given by
Poiseuille’s equation.
Ƞ= =
where,
P = Pressure difference between the two ends of the tube = hdg
h = height ; d = density ; g = acceleration due to gravity
r = radius of the capillary,
v = volume of the liquid,
l = length of the capillary tube,
t = time required for the flow.
If equal volumes of two different liquids are allowed to flow through the same capillary tube under
identical condition. Then relative viscosity is given by the expression,
ƞ tl Ⅹ dl liquid
= t Ⅹd
ƞ w w water
The flow times for the liquid and water are determined in Ostwald’s viscometer. Knowing the
densities of the liquid and water and also knowing the viscosity coefficient of water, viscosity
coefficient of liquid can be calculated. Since viscosity is dependent on temperature the measurement
can be carried out in water bath to reduce the change in temperature.
1
Procedure
1) To determine the density of given liquid :
(i) Fill the density bottle with liquid, avoiding bubbles. The ground neck should be covered to about
1/3.
(ii) In a thermostatic bath, adjust the temperature of the bottle and contents to 20 °C.
(iii)Align the stopper respectively, the thermometer of the density bottle according to the marking
and insert carefully. The capillary tube fills up and the displaced liquid comes out.
(iv) Carefully dry the outer surfaces of the stopper (respectively, the side capillary) and the density
bottle with tissue.
(v) Determine the weight of the filled density bottle.
(vi) Calculate the density from the mass (weight) and the volume of the liquid at the reference
temperature of 20 °C. The volume is engraved on the bottle. Use the following equation:
Density (ρ) = Mass (m)/Volume (V)
Take the buoyancy of the air into account for weighing.
Note: Calibrated density bottles have a unique identification number on all component parts. Only
use parts with the same number together.
Calculation
1. Weight of empty specific gravity bottle =……….g
2. Weight of liquid + specific gravity bottle =……….g
3. Weight of liquid =…………g
( )
Density = = ( )
= ………….
Therefore, the density of the given liquid = …………g/cm 3
2) To determine viscosity co-efficient of a given lubricant using Ostwald’s viscometer
Take a clean and dry Ostwald’s viscometer. Fix it vertically to a stand in a constant water bath (beaker
containing water). Transfer 20 cm3 of the given lubricant into the wider limb Ostwald’s viscometer
using a pipette. Suck the given liquid above the upper mark of the viscometer allow the liquid to flow
freely through the capillary. When the level of the liquid just crosses the upper mark start the stop
clock and stop the stop clock when the level of the liquid just crosses the lower mark of the
2
viscometer. Note the time of flow in seconds (t lubricant). Repeat the same procedure to get agreeing
values.
Pour out the liquid rinse the viscometer with acetone and dry it. Transfer 20 cm 3 of water into the
wider limb of the Ostwald’s viscometer, as described above note the time (t water) taken by water to
flow through the same distance in the viscometer thoroughly before conducting the experiment with
the test liquid and distilled water.
OBSERVATION & CALCULATIONS
Constant temperature water bath (thermostat) temperature =………..0C
To determine the flow time
Time of flow (seconds) Average time of flow

Trial 1 Trail 2 Trial 3
Given lubricant
Liquid (t l)
Water (tw)
where density of liquid = d liquid = ………. g/cm3
where density of water = dwater =…………g/cm3
Viscosity co-efficient of water = Ƞwater =………. milli poise
( Ⅹ )
Therefore, co-efficient of the liquid Ƞ liquid = Ⅹ Ⅹ ƞ
=……………. Milli poise
3
Result:
Viscosity co-efficient of the given lubricant =…………. Milli poise at……… 0C
4
Experiment – 8
C4. Estimation of sodium present in soil / effluent sample using flame
photometer
Aim : To estimate the amount of sodium present in given soil sample using flame photometry
Principle
Sodium, potassium and calcium and lithium and other common elements characteristic colors with
the Bunsen flame. The intensity of colored flame varies with the amount of element introduced. This
forms the basis of lame photometry.
When a solution containing a compound of the metal to be investigated is aspirated into flame, the
following processes occur:
i) Solvent evaporates leaving behind a solid residue.
ii) Vaporization of solid coupled with dissociation into its constituent atoms, which are initially in
ground state.
iii) Some gaseous atoms, which get excited by the thermal energy of the flame to higher energy
levels.
The excited atoms, which are unstable quickly, emit photons and return to lower energy state i.e.,
ground state. Flame photometry involves the measurement of emitted radiation.
N1/N0 = (g1/g0 ) eΔE/KT

N1 = Number of atoms in the excited state
N0 =Number of atoms in the ground state
g1/g0 = ratio of statistical weights for ground and excited states
ΔE = Energy of excitation = hν
K = the Boltzmann constant; T = Absolute Temperature
From the above equation, it is evident that the ratio N1/N0 is dependent upon both the excitation
energy E and the temperature T. An increase in temperature and a decrease in ΔE will both result in
a higher value for the ratio N1/N0.
Procedure
1) Transfer 2, 4, 6, 8, 10 ml NaCl solution (which is prepared by weighing accurately 1.271 g NaCl
into a 1-liter standard volumetric flask and dissolving the crystals and diluting the solution up to
5
the marks with distilled water and mixing the solution gives 1ppm Na/ml) into 50 ml standard
volumetric flasks and dilute up to the mark with distilled water.
2) Place the distilled water in the suction capillary of the instrument and set the instrument to read
zero.
3) Place each of the standard solutions in the suction capillary and set the instrument to read flame
emission intensity 2,4,6,8 and 10 respectively (rinse with distilled water between each reading)
using sodium filter 598nm.
4) Dilute the given test solution up to the mark with distilled water, mix well and place the solution
in the suction capillary and record the reading.
5) Draw a calibration curve by plotting the emission intensity (y axis) and volume of NaCl solution
(x-axis)
6) From the calibration curve, find out the volume of the given test solution and from which
calculate the amount of Na in the sample.
OBSERVATION AND CALCULATION :
Volume of sodium Concentration of sodium = Emission intensity

chloride solution 0.5mg Ⅹ volume of solution
(cm3)
5.0 5 ppm
10.0 10 ppm
15.0 15 ppm
20.0 20 ppm
Test solution
Sodium present in
soil/effluent
sample
1000 cm3 of stock solution contains 2.522 g of NaCl

58.5 g of NaCl =23.0g of Na
2.522 g of NaCl = (23 x 2.522) / 58.5
= 0.999 g of Na Per 1000 cm 3 of stock solution
6
Therefore 1 cm3 of NaCl = 0.999 = 0.999 Ⅹ 10-3 g = 0.999 mg

1000
Therefore, Na present in a cm3 of test solution = a cm3 x 0.999 mg =----------------- mg or ppm
Result:
The weight of Sodium present in the given soil / effluent sample = ---------------mg or ppm
Flame photometer
7
Schematic representation of flame photometer
8
Experiment – 9
C5. Determination of Chemical Oxygen Demand (COD) of Industrial
Wastewater Sample
Aim : To determine the chemical oxygen demand (COD) of given wastewater sample.
Principle
Chemical oxygen demand (COD) value is a measure of total oxidizable impurities present in the
sewage. This includes both, biologically oxidizable and biologically inert but chemically oxidizable
impurities in the water. COD is defined as the amount of oxygen required to oxidize both organic
and in-organic impurities into CO2 and H2O by strong oxidizing agent like acidic K2Cr2O7 in a liter
wastewater at 25oC. It is expressed in mg.dm-3 or ppm of oxygen.
A known volume of waste sample is refluxed with excess of K 2Cr2O7 solution in sulphuric acid
medium and in the presence of Ag2SO4 and HgSO4. K2Cr2O7 oxidizes all oxidizable impurities.
Ag2SO4 catalysis the oxidation of straight chain organic compounds, aromatics and pyridine. HgSO 4
avoids the interference of Cl- ions by forming soluble complex with them. In the absence of HgSO 4,
chloride ions precipitate silver ions as AgCl. The amount of unreacted K2Cr2O7 is determined by
titration with standard ferrous ammonium sulphate (Mohr’s salt) solution. The amount of K 2Cr2O7
solution consumed corresponds to the COD of the water sample. To calculate the COD, blank
titration without the wastewater sample is carried out.
Ferroin (1,10-phenonthrolein-iron (II) complex) is used as the indicator in the titration to detect the
end point. The indicator is intensely red in colour. Strong oxidizing agents oxidize the indicator to
iron (III) complex, which has a pale blue colour.
[ Fe(C12H8N2)3]3+ + e- ↔ [ Fe(C12H8N2)3]2+
Pale blue Deep red
As long as K2Cr2O7 solution is present in the solution, the indicator is in the oxidized from, imparting
blue colour to the solution. The solution becomes blue green as the titration continues due to the
formation of Cr (III) ions as result of reduction of Cr2O7 2- ions. When K2Cr2O7 is completely
exhausted in the solution, the oxidized from of the indicator gets to the reduced form, imparting
reddish brown colour to the solution. Therefore, the end point is marked by the colour change from
bluish green to reddish-brown. The end point is sharp only at high acid concentration and therefore,
the solution is kept at a very high acidity of H2SO4.
9
A standard solution of FAS is prepared by dissolving a known weight of the salt in a known
volume of the solution. A test tube of dil.H2SO4 acid is added during dissolution to prevent the
hydrolysis of the salt in the solution.
The reaction between Mohr’s salt and K2Cr2O7 can be represented as follows:
K2Cr2O7 + 4 H2SO4 → K2SO4 + Cr2(SO4)3 +4 H2O+3(O) → 1
2 FeSO4 + H2SO4 + (O) → Fe2(SO4)3 +3 H2O x 3 →2
K2Cr2O7 +6 FeSO4 +7 H2SO4 → K2SO4 + Cr2(SO4)3 + Fe2(SO4)3 +7 H2O
Equivalent weight of Mohr’s salt = Molecular weight = 392
Procedure:
(a) Preparation of standard FAS (Mohr’s) solution :
Weight accurately given FAS crystals transfer it into a 250 cm3 standard flask. Add a test tube of
dilute H2SO4 and little distilled water to dissolve the crystals. Make up it to 250 cm3 using distilled
water, shake well for uniform concentration.
(b) Determination of COD :
Pipette out 25 cm3 of the given waste sample into conical flask. Add 3/4th test tube of sulphuric acid
solution. Then add 10 cm3 of 0.1N K2Cr2O7 solution into the flask. Add 5-6 drops of ferroin indicator
and titrate against standard FAS solution till the colour changes from bluish green to reddish brown.
Repeat the titration for agreeing values.
Blank: (Blank titrate value (x) will be given)
Blank titration is performed by taking 25 cm3 distilled water in the place of wastewater.
OBSERVATION & CALCULATIONS :

I. Preparation of standard FAS (Mohr’s salt) solution:
Weight of weighting bottle + FAS crystals = W1=…………. g
Weight of empty weighing bottle = W2 =………………. g
Therefore, weight of FAS (Mohr’s salt) = (W1-W2) = W3…………… g
Therefore, normality of FAS solution = N FAS = Wt. of FAS taken (W3) Ⅹ 4
Eq.Wt. of Mohr’s salt (392)
10
= W3 x 4
392
NFAS =………….. N
II. Estimation of COD value:
Burette: Standard FAS solution.
Conical flask: 25 cm3 wastewater sample + 10 cm3 K2Cr2O7+ ¾th test tube of H2SO4 + 1 gm
Ag2SO4+ 1gm HgSO4 boil, cool
Indicator: Ferroin (1,10 phenanthroline ferrous sulphate)
End point: Bluish green to reddish brown
Burette level I II III
Final burette reading
Initial burette reading
Volume of FAS
(cm3)Consumed.
Volume of FAS consumed to react with 25 cm3 of wastewater y =…………. cm3

Given volume of FAS required for blank titration = x =…………ml
1000 cm3 of1N FAS = 1 equivalent of oxygen = 8 gm of Oxygen
Therefore, COD value = 8 (x-y) NFAS x1000
V wastewater
= 8(x-y) NFAS x 1000
25
= …………………….
COD value = ………………. mg/dm3 of oxygen.
Result:
COD of the given sample of wastewater = ……… mg / dm 3 of oxygen
11
Experiment - 10
D1. Evaluation of acid content in beverages by using pH
sensors and simulation.
Aim
To determine the acid content in various beverage samples using pH sensor.
The Effect of Acidity on Food

Acid may be present in foods and drinks naturally, developed during processes such as fermentation,
or added during processing as a standard means of preservation: pH values below 4.6 limit the growth
of microorganisms such as Clostridium botulinum, the causative agent of botulism. Therefore, acidity
testing is important throughout the entire food processing value chain.
pH Measurement
pH indicates a food or beverage’s degree of acidity or alkalinity. A pH meter measures this acid
strength in terms of the potential difference between a reference electrode (like Calomel or
Ag/AgCl) and a pH electrode (glass electrode). This difference is then related to the concentration
of H+ ions in the solution and corresponds to the acidity of the solution.
Foods and drinks display a broad range of pH values, which relate to the sample’s acidity or
alkalinity. Some foods such as meat, dairy products, alcohol, lemon juice, carbonated water, and
vinegar fall towards the acidic end of the pH spectrum, whereas common vegetables and fruits fall
towards the alkaline end, as shown in the following table
12
13
Experiment – 13
11
D3. Design an experiment to identify the presence of proteins in given
sample
Aim
To perform a total protein lab test for identifying the presence of proteins in the samples given.
Theory
Proteins possess a higher molecular mass of long-chain polymers that consist of α-amino acids. Cells
contain proteins and they are therefore present in all living bodies. Proteins consist of carbon, oxygen,
nitrogen, hydrogen, and often sulphur and phosphorus. There are a few tests that are carried out for
finding the presence of proteins in the samples given.
These laboratory tests of proteins are:
1. Biuret test
2. Millions test
3. Xanthoproteic test
4. Ninhydrin test
Procedure
The procedures of the laboratory test of proteins are as follows;

1. Biuret Test:
• Take the sample given that is to be tested in a test tube.
• Then add 2ml of the sodium hydroxide solution to the sample.
• To this add about 5 to 6 drops of the copper sulfate solution.
• If a bluish violet colour appears, it indicates the presence of the proteins.
2. Xanthoproteic Test:
• Take 2ml of the sample in a clean test tube.
• Add a few drops of the concentrated sulfuric acid to it and then heat.
• If a yellow precipitate is seen to be formed, it confirms the presence of the proteins.
3. Millions Test:
• Take 2ml of sample solution given in a test tube.
• To it add about 2–3 drops of the Millon’s reagent and then shake well.
14
• Observe any changes.

• If a white precipitate is seen which then changes to brick red when heated, then it confirms
the presence of the proteins.
4. Ninhydrin Test:
• Take the given sample solution that is to be tested in a test tube.
• Add about 1–2ml of the ninhydrin solution to it.
• Then boil the mixture and observe any changes.
• If the solution turns blue in colour, then it confirms the presence of the proteins.
15
BRIEF PROCEDURE
Expt No.1 : ESTIMATION OF TOTAL HARDNESS OF WATER BY EDTA
COMPLEXOMETRIC METHOD
Part A: Preparation of standard solution
Weigh out the given disodium salt of EDTA crystals accurately into a 250 cm 3 volumetric flask. Add
5 cm3 of ammonia. Dissolve in distilled water and dilute up to the mark, mix well.
.
Molarity of EDTA =
. . ( . )
Part B: Determination of total hardness

Burette: Standard Na2EDTA Solution.
Conical Flask: 25 cm3 water sample +5 cm3 buffer (Ammonium hydroxide–ammonium chloride
NH4OH – NH4Cl) solution.
pH maintained: around 10 (Buffer solution)
Indicator: Eriochrome black-T
Colour Change: Wine red to clear blue.
Conclusion / Result: From the volume of Na2EDTA solution consumed, calculate the total hardness
of the given water sample.
Expt No.2 : DETERMINATION OF COD OF WASTE WATER

Part A: Preparation of standard FAS solution (Mohr’s salt solution)
Weigh out the given FAS crystals accurately into a 250 cm3 volumetric flask. Add 2 test tube of dil
H2SO4. Dissolve in distilled water and dilute up to the mark, mix well.
Normality of FAS = Wt. of FAS taken (W3) Ⅹ 4
Eq.Wt. of Mohr’s salt (392)
Part B: Determination of COD of waste water sample.
Burette: Standard FAS Solution.
Conical Flask: 25 cm3 waste water sample +10 cm3 K2Cr2O7+ 3/4 test tube of 1:1 H2SO4 + 1g of
AgSO4 + 1g of HgSO4
Indicator: Ferroin (1,10-PHENANTHROLINE IRON(II) SULFATE COMPLEX)
Colour Change: Blush green to reddish brown.
Conclusion/Result: Perform the blank titration in the same way as above, without taking waste
water. From the difference of the titre values, calculate the COD of the given waste water sample.
16
Expt No.3 : CONDUCTOMETRIC ESTIMATION OF ACID MIXTURE USING

STANDARD NaOH SOLUTION
Pipette out 25 cm3 of acid mixture into a beaker. Immerse conductivity cell into it. Connect the cell
to conductometer and measure the conductance. Add NaOH solution in increment of 0.5 cm 3 and
measure the conductance after each addition. Plot the graph of conductance against volume of NaOH
and determine the equivalence point. Calculate the normality and weight of HCl and CH 3COOH in
the given solution.
V1 = Neutralization point of HCl

V2 = Neutralization point of CH3COOH
Expt No. 4 : DETERMINATION OF pKa VALUE OF VINEGAR

Pipette out 25 cm3 of the given vinegar into a beaker. Immerse the glass electrode and calomel
electrode assembly inti it. Connect the electrodes to the pH meter. Add NaOH from the burette in
increasement of 0.5 cm3 and determine the equivalence point. Plot a graph of pH against volume of
NaOH and another graph of ∆pH/∆V vs volume of NaOH. Using the graphs, determine pKa value of
the given weak acid.
∆𝐩𝐇 pKa Half equivalence

∆𝐕 point (Veq /2)
Volume of NaOH
17
Expt No.5 : ESTIMATION OF FERROUS AMMONIUM SULPHATE DING

STANDARD POTASSIUM DICHROMATE BY POTENTIOMETRIC
TITRATION
Pipette out 25 cm3 of FAS into a beaker. Add two test tubes of dilute H2SO4. Immerse calomel and
platinum electrode assembly into it. Connect the electrodes to a potentiometer and measure the
potential. Add K2Cr2O7 from the burette in the increment of 0.5 cm3 and measure the potential after
each addition. Plot the graph of ∆E/∆V against volume of K 2Cr2O7. Calculate the normality and the
weight of FAS in the given solution.
∆𝐄
∆𝐕
Equivalence point (X)
Volume of K2Cr2O7
Expt No.6 : COLORIMETRIC ESTIMATION OF COPPER USING OPTICAL

SENSOR
Transfer 2, 4, 6, 8, 10 cm3 of given copper sulphate solution into separate volumetric flasks. Add 5
cm3 of ammonia to each one of them and also to the given test solution of unknown concentration.
Dilute upto the mark using distilled water and mix well. Measure the absorbance of each of this
against blank (only ammonia and water) solution. Plot a graph of absorbance (OD) against volume
of copper sulphate and determine the concentration of the test solution. λ max for blue color = 620 nm.
18
Expt No.7 : DETERMINATION OF CO-EFFICIENT OF VISCOSITY OF A

LUBRICANT USING OSTWALD’S VISCOMETER.
Transfer 20 cm3 of the given liquid (organic) into a wider limb of the viscometer and suck the liquid
through the narrow limb. Determine the time of flow between two fixed points, one above and another
below of the bulb in the narrow limb of viscometer. Repeat and calculate the average time of flow.
Pour out the liquid (organic), and wash with acetone and dry it. Now transfer 20 cm 3 of water into
the wider limb of the viscometer and determine the average time flow for water as before. From the
density of the liquid, density of the water and viscosity coefficient of water determine the viscosity
of the given liquid (organic).
( Ⅹ )
Viscosity coefficient of liquid, Ƞ liquid = Ⅹ Ⅹ ƞ
19
VIVA VOCE QUESTIONS

DETERMINATION OF pKa OF Vinegar USING pH METER
1. How is pKa of a weak acid evaluated from the graph?
pH at half equivalence point gives the pKa of a weak acid
2. What is a weak acid?
Weak acids are weak electrolytes, which ionize incompletely in aqueous solution.
3. Give an example for weak acid?
Acetic acid, Oxalic acid, Formic acid
4. What is pKa of a weak acid?
pKa is defined as, negative logarithm to the base 10 of dissociation constant of weak
acid. i.e., pKa = - log10Ka, Where Ka is the dissociation constant of the weak acid.
5. What is meant by pH?
pH is defined as negative logarithm to base 10 of hydrogen ion concentration.
pH = - log10[H+]
6. Why glass electrode is called an ion selective electrode?
Because it is able to respond to certain specific ions (H+ ions) only and develop a
potential while ignoring the other ions in a solution.
7. How is the measurement of pH made?
The measurement of pH is made by determining the emf of the cell containing glass
electrode and the calomel electrode immersed in the test solution. The emf of the cell
is expressed by the equation E = K + 0.0591 pH, where K is a constant.
8. How are pH and pKa related?
According to Henderson-Hasselbalch equation, pH = pKa + log10 [salt] / [acid]
9. Why pH at half equivalence point is equal to pKa?
At half equivalence point concentration of salt = concentration of acid, Therefore
pH = pKa
10. How are pKa and strength of a weak acid related?
Higher the pKa, lower will be the strength of the weak acid.
20
11. What are the electrodes used in the measurement of pH and determination of
pKa?
Glass electrode (indicator electrode) and calomel electrode (reference electrode).
In this case, glass electrode acts as anode & calomel acts as cathode.
12. Why is pH increases suddenly after the equivalence point?
At the equivalence point, all the weak acid has been neutralized by the base.
Afterwards the concentration of hydroxyl ions increases. So, pH increases suddenly.
13. What is strong acid?
The substance which ionise almost completely into ions in aqueous solution.
Eg: HCl, H2SO4, HNO3.
14. What is degree of ionisation?
No of molecules of the electrolyte which ionises
Degree of ionisation = ---------------------------------------------------------------
Total no of molecules of electrolyte
15. What is Ka?
Ka is the dissociation constant of a weak acid.
[H3O+] [CH3COO-]
Ka(CH3COOH) = ------------------------------------
[CH3COOH]
POTENTIOMETRIC TITRATION - ESTIMATION OF FAS USING

STANDARD POTASSIUM DICHROMATE SOLUTION
1. What is single electrode potential?
The potential that is developed when an element is in contact with a solution containing
its own ions is called single electrode potential
2. What is standard electrode potential?
The potential that is developed when an element is in contact with a solution containing
its own ions in 1M concentration at 298 k is called standard electrode potential
3. What is meant by emf?
21
EMF is potential difference required to drive current across the electrodes.

EMF = Ecathode - Eanode
4. What is potentiometer?
It is a device or circuit used for measuring the emf between the two electrodes
5. What is potentiometric titration?
It is the measurement of emf to determine the concentration of ionic species in solution
is called potentiometry
6. What is the principle of potentiometric titration?
The measurement of the emf between two electrodes (indicator and reference) and to
determine the equivalence point of redox reaction
7. Which are the electrodes used in potentiometric electrode?
Platinum electrode as indicator electrode (anode) and calomel electrode as reference
electrode (cathode)
8. What is determining factor in the oxidation-reduction reaction?
The determining factor is the ratio of the concentrations of the oxidized and reduced
forms.
9. What is indicator electrode?
The indicator electrode is an electrode whose potential is dependent upon the
concentration of the ion to be determined. Ex: Platinum electrode
10. What is the reaction occurring between FAS and potassium dichromate?
6FeSO4 + 7H2SO4 + K2Cr2O7 → 3Fe2(SO4)3 +K2SO4 + Cr2(SO4)3 + 7H2O
Acidified potassium dichromate oxidizes ferrous sulphate to ferric sulphate and itself
gets reduced to chromic sulphate
11. Why sulphuric acid is added to FAS solution during emf measurement?
In presence of sulphuric acid, potassium dichromate oxidizes ferrous ion (Fe+2) to
ferric ion (Fe+3)
12.Why the colour of the solution changes to green on adding potassium
dichromate?
Due to formation of green coloured chromic sulphate.
13. Why emf rapidly change at the equivalence point?
22
At the equivalence point, emf depends on concentration of both ferric ion and
dichromate ion. Therefore, emf rapidly change at the equivalence point.
14. What are the advantages of potentiometric titrations?
i) Turbid, fluorescent, opaque or coloured solutions can be titrated
ii) Mixture of solutions or very dilute solutions can be titrated.
iii) The results are more accurate
COLORIMETRIC DETERMINATION OF COPPER USING OPTICAL

SENSOR
1. What is the basic principle of colorimetric measurements?
It consists of comparing under well-defined conditions, the colour produced by the
substances in amount with the same colour produced by a known amount of material
being determined.
2. What is colorimetry?
Chemical analysis through measurements of absorption of light radiation in the visible
region of the spectrum (400-760nm) with respect to a known concentration of the
substance is known as colorimetry
3. What forms the basis for colorimetric determination?
The variation of colour of a system with change in concentration of some component
forms the basis for the colorimetric determination
4. What is photoelectric colorimeter?
It is an electrical instrument, which measures the amount of light absorbed using a
photocell.
5. What are filters? Why are they used?
The filter consists of either thin film of gelatin containing different dyes or of coloured
glass.
The filters are used in colorimeter for selecting any desired spectral region.
6. What is wavelength?
The distance between any two successive peaks or troughs of waves is called wave
length. It is represented by λ
7. What is wave number?
23
It is reciprocal of wavelength. Wave number = 1/ λ = Frequency / Velocity of light

8. What is frequency?
It is the number of waves passing through a point per second. It is represented by ν
9. State Beer’s law.
The intensity of a beam of monochromatic light decrease exponentially as the
concentration of the absorbing substance increases arithmetically.
10. State Lambert’s law.
When a monochromatic light passes through a transparent medium, the rate of
decrease in intensity with the thickness of the medium is proportional to the intensity
of the light. or the intensity of the emitted light decreases exponentially as the thickness
of the absorbing medium increases arithmetically.
11. State Beer-Lambert’s law.
The amount of light absorbed is directly proportional to the concentration and path
lenth of the solution.
A = log I0 / It = єcl ;(Є = Molar extinction coefficient, c = concentration, l = path
length)
Therefore, A α C
12. What is calibration curve?
It is the plot of absorbance or Optical Density against concentration of solutions. For
solutions obeying Beer’s law, this is a straight line.
13. What is meant by transmittance?
It is the ratio of amount of light transmitted (It) to the total amount of light absorbed
(I0)
T = It / I0
Absorbance = 1 / T = I0 / It
14. What is absorbance or optical density?
Reciprocal of transmittance, I0/It is called absorbance or optical density
A= log10 = log1/T= -logT
15. How is optical density is related to the concentration of the substance?
The optical density is directly proportional to the concentration of the substance
24
16. What is a stock solution?

A stock solution is a standard solution in which a known amount of solute dissolved
in a known volume of solvent.
17. Can different nessler’s tubes be used during OD measurements of solutions?
No, because absorbance depends on the path length of the solution.
18. Mention a few advantages of photoelectric colourimetric determinations?
i) A colourimetric method will often give more accurate results at low
concentrations than the corresponding titrimetric or gravimetric procedure.
ii) A colorimetric method may frequently be applied where no satisfactory
gravimetric or titrimetric procedure exits i.e. for certain biological substance.
19. Why are different volumes of solution taken in the flask?
Different volumes of solutions are taken to prepare standard solutions of different
concentration, which are used to plot a calibration curve.
20. What is blank solution?
A blank solution is identical in all respect to the test solution except for the absence of
test solute.
21. Why is a blank solution used in colorimetric estimation?
To nullify the absorbance caused due to the colouring impurities present in the
reagents.
22. Name the complex obtained when ammonia is treated with copper sulphate
solution?
Cuprammonium sulphate, [Cu (NH3)4]SO4 a dark blue colour complex
23. Why is ammonia added? Why is that same amount of ammonia added?
25
Ammonia is added to get cuprammonium sulphate [Cu(NH3)4]SO4 a dark blue

complex.
Same amount of ammonia is added to nullify the absorbance due to any colouring
impurities present in ammonia.
24. Why is estimation of copper done at 620 nm wave length?
The estimation of copper is carried at 620 nm wave length because the complex shows
maximum absorbance at 620 nm.
25. Mention a few important criteria for a satisfactory colorimetric analysis?
i) In order to obey Beer-Lambert’s law, the solute must not undergo salvation,
association, dissociation, hydrolysis or polymerization in the solvent used.
ii) The colour produced should be sufficiently stable to permit an accurate reading to
be taken.
iii) Clear solutions free from traces of precipitate or foreign substances in either blank
or standard test solution should be used.
CONDUCTOMETRIC ESTIMATION OF ACID MIXTRE USING STD. NaOH

SOLUTION.
1. What is conductivity of an electrolyte solution?
Is a measure of its ability to conduct electricity?
2. What is conductance?
Reciprocal of resistance is called conductance.
3. What is a cell?
A device, which produces an EMF and delivers electric current as the results of a
chemical reaction.
4. What factors determine the conductance of a solution?
Two factors determining the conductance of a solution are;
1. Mobility of ions (Higher the mobility, higher is the conductance) and
2. Number of ions (More the number of ions, more is the conductance).
5. What is cell constant?
26
Is a function of the electrode areas, the distance between the electrodes and the
electrical field pattern between the electrodes. Cell constant is defined as the ratio of
the distance between the electrodes, d, to the electrode area, A.
6. What is the unit of cell constant?
Commonly, expressed in cm-1
7. State Ohm’s law?
Current, I (ampere), flowing in a conductor is directly proportional to the applied
electromotive force, E (volt) and inversely proportional to the resistance R (ohm) of
the conductor. I = E/R.
8. What is the unit of conductance?
Ohm-1m -1 or Sm-1 (S- siemens).
9. Mentions the different types of conductance?
i) Specific conductance. ii) Equivalent conductance iii) Molar conductivity.
10. Which of the above conductivity is measured during the conductometric
titration?
Specific conductance.
11. What is specific conductivity?
Conductivity of a solution between 1cm2 area and kept 1 cm apart.
12. What is equivalent conductance?
Conductivity of a solution, which contains 1g equivalent of solute, when placed
between 2 electrodes of 1cm apart. λ = kV.
13. What is molar conductivity?
Conductivity of the solution, which contains 1g molecular weight of a substance, when
placed between two electrodes of 1 cm apart, µ = kV.
14. What is the principle involved in conductometric titration?
There is a sudden change in conductance of a solution near the end point. Hence the
end point is determined graphically by plotting conductance against the titer values.
Measuring resistance and the dimension of conductivity cell (Ohm law) and plotting
the titration curve (conductance-as reciprocal of resistance against the volume of
titrant) is the principle.
15. Explain the variation in conductivity at the end point?
27
In the case of NaOH and HCl experiment, addition of NaOH to HCl decreases the
conductance because of the replacement of high conducting mobile H + ions
(Conductivity: 350 Ohm-1m -1) by the less mobile Na+ ions (Conductivity: 50 Ohm-1m
-1
). Trend continues till all the hydrogen ions are replaced and end point is reached.
Further addition of NaOH, increases the conductance because of the presence of free
OH- ions (Conductivity: 198 Ohm -1m -1).
16. Why are the slopes of curves before and after neutralization point not exactly
the same?
Before the neutralization point, the conductivity is mainly due to the highly mobile H +
ions and after the end point, it is mainly due to OH- ions, which are less mobile
compared to H+ ions. As a result, magnitude of decrease in conductivity is more before
the neutralization point compared to that after the neutralization point.
17. How is the accuracy of the method determined?
Accuracy of the method is greater when the angle of intersection is more acute and
more nearly the end points of the graph on a straight line.
18. What are the advantages of conductometric titration over visual
potentiometric titrations?
i). Accurate for both dilute and concentrated solutions.
ii). Can be employed for coloured solutions.
iii). Very weak acids such as boric, phenol (cannot be titrated potentiometrically) can
be titrated.
iv). Mixture of acids can be titrated more accurately.
DETERMINATION OF VISCOSITY COEFFICIENT OF A GIVEN

LUBRICANT USING (OSTWALD’S VISCOMETER)
1. What is viscosity?
Viscosity arises due to internal friction between moving layers of molecules. A moving
layer exerts a drag or friction on its nearest moving layer backward. This property of
a liquid by which it retards or opposes motion between the layer is called viscosity.
2. What is viscosity co-efficient of a liquid?
The viscosity coefficient of a liquid is defined as the tangential force per unit urea
required to maintain a unit velocity gradient between any two successive layers of a
liquid situated unit distance apart.
28
3. What is density of liquid?

The density of a liquid is the mass of its unit volume.
4. The density of a substance is expressed relative to what?
The density of a substance is expressed relative to that of water at 40C
5. What is specific gravity?
Specific gravity or relative density is the weight of a given liquid divided by the weight
of an
equal volume of water at the same temperature.
6. How are specific gravity and density of liquid related?
Density of liquid = specific gravity of the liquid x Density of water at the same
temperature
7. What is the SI unit of viscosity coefficient?
Pascal second (1 ps = 1 kg m-1 s-)
8. What is the unit of viscosity coefficient in cgs system?
Millipoise.
9. What are the factors that affect the viscosity of a liquid?
i) Increase in molecular weight results in an increase in viscosity.
ii) Branched chain compounds have higher viscosity than those involving straight
chain compounds.
iii) The polar compounds are more viscous than the non-polar ones. The presence of
hydrogen bonds cause the viscosity to increase.
iv) The viscosity of liquids increases by the presence of lyophilic colloids and
suspended impurities.
v) Temperature has marked influence on the viscosity of a liquid (about 2% per
degree).
10. What is the law based on the viscous flow of liquids through capillary tubes?
Poiseuille law
η = Πρr4t / 8Vl
V = volume of the liquid, r = radius of the tube, l = length of the tube,
29
ρ = pressure difference between two ends of the tube,

η = the coefficient of viscosity of the liquid,
t = time required for the volume.
11. How does viscosity vary with temperature?
The viscosity of a liquid usually decreases with rise in temperature.
12. Why should the viscometer be dried before the measurements are done?
The viscometer should be dried to avoid the formation of emulsion, which changes the
rate of flow of the liquid.
13. Why is acetone used for cleaning viscometer?
Acetone is volatile organic liquid. To dry the viscometer quickly, it is rinsed with
acetone.
14. Why is viscometer not rinsed with the given liquid or water?
If the viscometer is rinsed with given liquid or water before measuring the flow time,
the volume taken will be more than a definite known volume.
15. Why do you require laboratory temperature for viscosity determination?
Because the physical constants like density and viscosity of a liquid vary with
temperature.
16. How is the viscosity of a liquid related to its mobility?
Viscosity of a liquid is inversely proportional to its mobility.
17. What is fluidity of a liquid?
Fluidity of liquid is the reciprocal of viscosity co-efficient. It is a measure of the ease
with which the liquid flows.
Fluidity (Ө) = 1/ η, η = the viscosity co-efficient.
ESTIMATION OF TOTAL HARDNESS OF WATER BY EDTA METHOD

1. Why buffer (NH4OH + NH4Cl) added?
Buffer is added to maintain a pH of 10. Otherwise pH decreases as H + ions are released due to the
substitution of metal ions for H+ ions in EDTA.
2. What is hard water?
30
Hard waters are a kind of water that requires considerable amounts of soap to produce foam and
lather.
3. What is total hardness of water?
The sum of both temporary and permanent hardness is called total hardness of water.
4. How are the waters classified based on the degree of hardness?
Soft water 0 to 75 mg / litre
Moderately hard water 75 to 150 mg / litre
Hard water 150 to 300 mg / litre
Very hard water > 300 mg / litre
5. How is hardness of water caused?
Hardness of water caused by divalent metallic cations in association with anions such as HCO3- SO42-
, Cl-, SiO32- etc. the principal hardness causing cations are calcium and magnesium.
6. What is the difference between temporary and permanent hardness?
Temporary hardness is due to unstable bicarbonates (HCO3-) of Ca and Mg, while permanent
hardness is due to more stable Cl – and SO42- of Ca and Mg
7. How temporary hardness is be removed?
The temporary hardness of water can be removed by boiling water during which bicarbonates
decomposes to give carbonates.
8. How do you express the total hardness of water?
It is expressed as parts per million of CaCO3.
9.What is the full form of EDTA?
Ethylene diamine tetra acetic acid.
10. Write a structural formula of EDTA?
11. How many replaceable hydrogen atoms are present in disodium salt of EDTA?
Two
12. Why is disodium salt of EDTA preferred to EDTA?
Because EDTA is sparingly soluble in water.
13. Why is ammonia solution added while preparing EDTA solution?
Because to increase the rate of dissolution of EDTA salt.
31
14. What is buffer capacity?

The capacity of a solution to resist the change in pH
15. Give an example of acidic buffer?
CH3COOH + CH3COONa
16. Give an example of basic buffer?
NH4OH + NH4Cl
17.What is buffer solution?
The solution which resists change in its pH value even after adding small amounts of an acid or base
to it.
18.What is the chemical name of EBT?
Eriochrome black-T
Sodium 4-[(1-hydroxynaphthalen-2-yl-hydrazinylidene]-7-nitro-3-oxo-Y-naphthalene1-sulfonate.
19. Why is EBT shows wine red at the beginning and blue colour at the end?
EBT is blue in colour, which is added to hard water with a pH of 10; it combines with a few of the
calcium and magnesium ions to form a weak complex which is wine red in colour as shown in the
equation.
M 2+ + EBT → M-EBT , (Wine red complex)
M-EBT + EDTA → M-EDTA + EBT
(Blue) (Stable complex)
This action frees the EBT from the complex (M-EBT), and the wine red color changes to a blue
colour at the end of titration.
20. Titrations involving EDTA carried out slowly towards the end point. Justify?
Because the rate of formation of the metal complex of EDTA is very slow.
21. What is the application of hardness data in environmental engineering practice?
i) Hardness of water is an important consideration in determining the suitability of a water for
domestic and industrial uses.
ii) Determination of hardness serves as a basis for routine control of softening processes.
22. Structure of disodium EDTA?
32
DETERMINATION OF CHEMICAL OXYGEN DEMAND (COD) OF THE

INDUSTRIAL WASTE WATER SAMPLE
1. What is sewage?
Sewage is commonly a cloudy dilute aqueous solution containing human & household waste,
industrial waste, ground waste, street washings. Sewage contains organic and inorganic matters in
dissolved, suspended & colloidal states.
2. What is meant by industrial sewage?
The waste water coming out of industries such as chemical plant, fertilizer industries, leather
tanneries, sugar and paper industries, breweries, textile mills, oil refineries, pharmaceutical units are
called industrial sewage.
3. What is COD?
It is amount of oxygen required for the complete chemical oxidation of both organic and inorganic
matter present in the sample of water by a strong chemical oxidizing agent such as acidified
potassium dichromate.
4. What are the compounds present in industrial waste water sample?
Waste water contains organic impurities which include straight chain aliphatic compounds aromatic
hydrocarbons, straight chain alcohols, acids and other oxidizable materials.
5. What is BOD?
It is the amount of oxygen required for the complete oxidation of organic matter present in a liter of
waste water over period of 5 days at 200C.
6. Why COD greater than BOD value?
Because in COD both organic & inorganic matter get oxidized & in BOD only organic matters gets
oxidized.
7. What are end products of oxidation?
CO2 & H2O.
8. Why H2SO4 is added to conical flask?
Because Potassium dichromate acts as an oxidizing agent in presence of H 2SO4.
9. What is the unit of COD?
33
mg/litr of O2 or mg/dm3 of O2 or ppm of O2.

10. Name the oxidizing agent?
Potassium dichromate.
11. Explain the colour change during the titration?
Ferroin indicator is red in colour in the reduced form with the composition, [Fe(O-Phen) 3]2+ (ferroin),
When ferroin is added to conical flask containing waste water & potassium dichromate. The indicator
gets oxidized by potassium dichromate (oxidizing agent) to form [Fe(O-Phen) 3] 3+(ferriin), which is
bluish green. This solution is titrated with FAS taken in the burette (reducing agent) which reduces
ferrin to Ferroin which is in red colour which is the end point of titration.
Ferroin Red in color Ferrin Bluish green color
12. What is back titration?

Back titration is a technique used to find the concentration of the reactant by reacting with an excess
volume of reactant of known concentration.
13. Differentiate between blank & back titration. Why blank value is higher than back value?
Blank titration is done using distilled water instead of test solution (waste water) and back titration
is done using waste water as one of the solvents. Blank titration involves no oxidation of organic
matter.
14. What general groups of organic compounds are not oxidized in the COD test?
Aromatic hydrocarbons and pyridine are not oxidized in COD test.
15. What is the role of silver sulphate?
Silver sulphate acts as a catalyst in the oxidation of straight chain aliphatic hydrocarbons and acetic
acid. Oxidation is effective in presence of silver ions.
16. What is the role of mercuric sulphate?
Chloride ions normally present in high concentration in waste water undergo oxidation in COD test
and cause erroneously high results. Mercuric ions of mercuric sulphate bind the halide ions present
in waste water to form poorly ionized mercuric chloride and prevent the precipitation of silver halide
by making halide ions unavailable.
17. What are the products formed after COD analysis?
34
During COD analysis organic matter is completely oxidized to carbon dioxide and water by acidified
potassium dichromate solution.
18. Why is sulphuric acid added during the preparation of std. FAS solution?
Sulphuric acid is added to prevent the hydrolysis of ferrous sulphate into ferrous hydroxide.
19. What is the composition of ferroin?

Ferroin is ferrous 1, 10-Phenanthroline sulphate.
20.Why blank titration is necessary?

Because the COD measures the oxygen demand in the sample of water, it is important that no outside
organic material be accidental added to the sample to be measured. To control for this, so called blank
sample is required.
21. Mention a few applications of COD test in environmental engg.?
i) The COD test is extensively used in the analysis of industrial wastes
ii) It is particularly valuable in survey designed to determine and control losses to sewer systems
iii) The COD is helpful in indicating toxic conditions and the presence of biologically resistant
organic substances.
22. What is the limitation of COD?
One of the chief limitations of COD test is inability to differentiate between biologically oxidizable
and biologically inert organic matter. Also, it does not provide any evidence of the rate at which the
biologically active material would be stabilized under conditions that exits in nature.
35
THANK
YOU
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LABORATORY MANUAL

ENGINEERING CHEMISTRY for CSE

ATRIA INSTITUTE OF TECHNOLOGY

A – Demonstration (any two) offline/virtual:

To be a better analyst, understand the theory of the experiments you conduct.

Instructions for Volumetric Analysis

𝐹𝑒2+ + 2𝐹𝑒3+ + 8𝑂𝐻− 𝐹𝑒3𝑂4 + 4𝐻2𝑂

1) Pipette out 25 cm3 of acid mixture in a 250 ml beaker.

OBSERVATION & CALCULATION

Burette: 0.5 N NaOH solution

Volume of NaOH Conductance

6.5 (V2 - V1 ) = Volume of NaOH required to

(NV) HCl = (NV) NaOH

Weight of CH3COOH/ litre of solution = NCH3COOH x Eq. wt. of CH3COOH (60)

(i) Normality of HCl = NHCl =………………….. N

(ii) Normality of CH3COOH = NCH3COOH …………….. N

(iii) Amount of HCl per litre of solution = …………….. g/litre

(iv) Amount of CH3COOH per litre of solution = ………….. g/litre

E= E0 + 2.303 RT log (Fe3+)

1) Pipette out 25 cm3 of ferrous ammonium sulphate into a beaker.

OBSERVATION AND CALCULATIONS

Burette: 0.5 N K2Cr2O7 solution

0.0 ---------- -------- ----------

Equivalence point (X)

1. Normality of the given FAS solution = NFAS = ………….. N

CH3COOH + H2O → CH3COO- + H3O+

Therefore pKa = -log Ka

OBSERVATION & CALCULATION

Volume of pH ∆V ∆pH ∆𝐩𝐇

According to Henderson-Hasselbalch equation.

∆𝐩𝐇 pKa Half equivalence

Half equivalence point is = =…………………ml

Therefore, from graph (1) at half equivalence, pH = pKa =………..

Molecular weight of disodium salt of Na2EDTA = 372.24

(a) Preparation of standard solution of Na2EDTA :

(b) Determination of total hardness of water:

OBSERVATION & CALCULATIONS

II. Determination of total hardness of water:

Initial burette reading

Volume of Na2EDTA (cm3)

Volume of Na2EDTA consumed = V Na2EDTA =………….cm3

Therefore, Io=Ia + Ir+ It

For glass-air Ir is negligible, therefore Io= Ia+It

A = Log (Io/It) = €cl

Cu2+ + 4NH3 → [Cu (NH3)4]2+ (Deep blue)

OBSERVATION & CALCULATION

Flask No. Absorbance

2 4 cm3+5 ml.NH3 + H2O

3 6 cm3+5 ml.NH3 + H2O

4 8 cm3+5 ml.NH3 + H2O

5 10 cm3+5 ml.NH3 + H2O

249.54 g of CuSO4 contains 63.54 g of Cu

1000 cm3 of stock solution 2.037 g of copper

2. Weight of copper (II) present in electroplating effluent =………….. mg/litre

1) To determine the density of given liquid :

Take the buoyancy of the air into account for weighing.

2. Weight of liquid + specific gravity bottle =……….g

3. Weight of liquid =…………g

Therefore, the density of the given liquid = …………g/cm 3

2) To determine viscosity co-efficient of a given lubricant using Ostwald’s viscometer