Engineering Chemistry

(CHY1701)

Lab Manual

Name:
Reg. No.
Slot:
Semester: Winter Semester 2019 ~ 20
Faculty Name:

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 Instructions to the students

 Students are strictly advised to use googles, lab coat and shoes while inside the lab.
 The experiment that will be performed in the next approaching week will be
intimated to the students by the faculty.
 Students are advised to come prepared for the experiment before entering the lab.
The softcopy of the manual will be available either in FFCS (Course page) or
Moodle.
 All the observations should be hand written with pen and should be attested by the
faculty after performing the experiment.
 The evaluation of the experiment will be strictly based on the error values as shown
below.
 The evaluation of the experiments should be completed before doing the next
experiment, failing which marks shall be deducted by faculty.
 Students who were absent for the lab classes for genuine reasons (OD/death in the
family/health issues), shall be considered for repetition labs, only upon producing
the proper evidence / proof. In any case, the evaluation will be done only for a
maximum of 7 marks instead of 10.

Evaluation pattern:
For titration experiments:
Error Marks for skill Marks for presentation Total
0<1% 5 5 10
>1 < 2 % 4 5 9
>2 < 3 % 3 5 8
>3 < 4 % 2 5 7
>4 < 5 % 1 5 6
>5 0 5 5

For instrument related experiments:

Error Marks for skill Marks for presentation Total
0<2% 5 5 10
>2 < 4 % 4 5 9
>4 < 6 % 3 5 8
>6 < 8 % 2 5 7
>8 < 10 % 1 5 6
>10 % 0 5 5

CAM: Experiments = 50 M; Viva = 10 marks (Weightage = 60 M)

FAT: Marks distribution = 40 M (Experiment) + 10 M (Explanation of concept) = 50
M. (Weightage = 40 M).

2
 Instructions for performing experiments
Non-instrument based experiments:
Burette
1. Clean the burette with tap water and then rinse with distilled water
2. Rinse the burette with a small quantity of the solution to be filled in the burette
and discard the solution into the sink.
3. Fill the burette with required solution using funnel, remove the funnel and fill
the nozzle of the burette with the solution.
4. When the burette reading is noted down, the burette should be at the level of the
eye to avoid parallax error.

Pipette
1. Clean the pipette with tap water and then rinse with distilled water
2. Rinse the pipette with a small quantity of the solution to be pipetted and discard
the solution in to the sink
3. Pipette out exactly 20mL of the solution into a clean conical flask.
4. During transferring the solution into a clean conical flask, when all the solution
from the pipette runs out, touch the tip of the pipette to the bottom of the flask
gently.

Conical Flask
Clean the conical flask with tap water and then rinse with distilled water.
Test solution
1 Test solution is provided in a small reagent bottle. Transfer the given test
solution into a clean 100 mL volumetric flask using funnel, after complete
transfer of the test solution, add small amount (2-3 mL) of distilled water into
the reagent bottle and transfer this solution into the standard flask and finally
dilute the solution up to the mark using distilled water with utmost care.
Use this as test solution for estimation.
2. Test solution will be provided only one time.

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Titration
During the addition of the solution from the burette, the conical flask must be
constantly rotated with one hand while the other hand controls the stop cock of the
burette.

Instrument based experiments:

1. Instrument based experiments will be done by a group of students and each group can
have maximum of 2 students.
2. The groups will be made as per attendance order or as per faculty allotment.
3. Calibration of instruments is not given as part of the procedure and hence students
should follow instructions during the lab sessions.
4. Each student in a group should complete the experiment and submit the results.

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Exp.
DATE EXPERIMENT TITLE Marks /10
No.

Student signature Faculty Signature

5
Experiment: 01 Date

Water Purification: Hardness Estimation by EDTA method and its Removal

using Ion-exchange Resin
1. Introduction to Hard Water and its Classification: Water described as “hard” contains high
levels of dissolved Ca2+ and Mg2+ ions. Ground and surface water dissolve the Ca2+/Mg2+
containing ores/minerals from the surrounding soil and are enriched with these cations. Hardness
is commonly expressed as milligrams of CaCO3 equivalents per litre. Water containing hardness
causing species at concentrations below 60 mg/L are generally considered as soft; 60–120 mg/L
as moderately hard; 120–180 mg/L as hard; and more than 180 mg/L as very hard water. Based
on the type of anions associated with Ca2+/Mg2+ ions, the hardness is categorized as permanent
(non-carbonate) & temporary (carbonate) hardness.

2. Problems caused by Hard Water: Hard water can cause breakdown of boilers, cooling
towers and plumbing. When hard water is heated, the hardness causing salts tend to precipitate
out of solution, forming hard scale or soft sludge in pipes and surfaces. This can cause chocking
of pipes and restrict the flow of water. In boilers, the scale prevents efficient heat transfer
resulting in energy loss and overheating thereby paving way for serious accidents. At domestic
level, hard water reduces the effectiveness of soap by forming scums/precipitates, which adhere
to human skin. Human consumption of water containing excess of Ca and Mg are associated
with increased risks of osteoporosis, nephrolithiasis, colorectal cancer, hypertension, stroke,
coronary artery disease, insulin resistance, diarrhea and obesity.

3. Estimation of Hard Water: Traditionally, hardness in water is estimated by complexometric

titration using sodium salt of EDTA and EBT as indicator at pH = 9-10. EBT forms an unstable
wine-red colored complex with Ca2+/Mg2+ ions, which upon titrating with EDTA, results in the
breaking of weakly stable EBT-Ca2+/Mg2+ and formation of stable EDTA-Ca2+/Mg2+ complex.
The endpoint changes from wine-red (EBT-Ca2+/Mg2+) to steel blue (free EBT).

4. Modern Treatment of Hard Water: Hard water is made soft by the use of a water softener
i.e., ion-exchange resins (IER) which are very small porous spherical polymeric beads, with
specific functional groups (sulphonic/carboxylic acid) attached to the polymeric backbone.
Therefore, the IERs carrying a negatively charged exchange site can hold a positively charged

6
ion. When the hard water is passed through the resin beads, Ca2+/Mg2+ ions are exchanged from
the solution for hydrogen/sodium ions, which are much more soluble and does not precipitate out
to form scale or sludges. Eventually, the resin beads get saturated with hardness causing ions and
the exhausted beads are regenerated by using a mild acid or brine solution to flush out the
Ca2+/Mg2+ ions retained in the resin beads.

Hardness of water is due to the presence of dissolved calcium and magnesium

Problem
salts in water. EDTA forms stable complex with hardness causing salts and is
definition
used in the removal of scale and sludge forming impurities in industrial boilers.
EBT indicator-Metal ion complex is weaker compared to EDTA-metal ion
Methodology complex. The end point is the color change from wine red (EBT-Metal ion
complex) to steel blue (free EBT indicator).
Estimation of Calcium hardness (in ppm) in the given unknown sample.
Solution
Understanding the water softening using ion-exchange resins.
Student Students will learn to
learning a) perform complexometric titration
outcomes b) understand the efficiency of ion-exchange resins using in water purifiers

Principle: Ethylenediaminetetraacetic acid (EDTA) forms complexes with a large number of

cations including Ca2+ and Mg2+ depending upon the pH of solution. Hence, it is possible to
determine the total hardness of water using EDTA solution. EDTA in the form of its sodium salt
(H2Y2-) is commonly used in complexometric titration for estimation of metal ions because pure
EDTA (H4Y) is sparingly soluble in water. EDTA has six binding sites (the four carboxylate
groups and the two amino groups) providing six pairs of electrons. The resulting metal-ligand
complex, in which EDTA forms a cage-like structure around the metal ion, is very stable at
specific pH. All metal-EDTA complexes have a 1:1 stoichiometry. The H2Y2- form complexes
with metal ions as follows.
M + H2Y2- → MY2- + 2H+ ----------- (1)
Where, M is Ca2+ and Mg2+ present in water. Reaction (1) can be carried out quantitatively at pH
10 using Eriochrome Black T (EBT) as indicator. EBT forms a wine-red complex with M2+ ions
which is relatively less stable than the M2+-EDTA complex. On titration, EDTA first reacts with
free M2+ ions and then with the metal-EBT indicator complex. The latter gives a colour change
from wine-red to steel blue at the equivalence point.

Removal of hardness using ion exchange resins: Ion exchange is a reversible process. When
hard water is passed through cation-exchange resins packed in a narrow column, Ca2+ and Mg2+

7
cations in hard water are exchanged with Na+ or H+ ions in the resins. The exhausted resins can
be regenerated by passing brine solution or 10 % dil. HCl through the column. A typical example
of application is preparation of high-purity water for power engineering, electronic and nuclear
industries and in household water purifiers.

Requirements:
Reagents and solutions: Standard hard water (1 mg/mL of CaCO3 equivalents), 0.01 N EDTA
solution, EBT indicator, hard water sample, NH3-NH4Cl buffer solution and ion exchange resin.

Apparatus: Burette, pipette, conical flask, standard flask burette stand and ion exchange
column.

Procedure:
Titration-I: Standardization of EDTA
Pipette out 20 mL of the standard hard water containing 1mg/mL of CaCO 3 (1000 ppm) into a
clean conical flask. Add ~3 mL of ammonia buffer (NH4OH – NH4Cl) solution to maintain the
pH around 10. Add three drops of Eriochrome Black – T (EBT) indicator and titrate it against
the given EDTA solution taken in the burette. The end point is change of colour from wine red to
steel blue. Repeat the titration for concordant titre values. Let ‘V 1’ be the volume of EDTA
consumed.

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 S. Volume of standard hard water Burette reading (mL) Volume of EDTA
No. (mL) Initial Final (V1, mL)
1

Concordant titer value

Calculations:

20 mL of given hard water consumes V1 mL of EDTA

20 mg of CaCO3 requires V1 mL of EDTA for complexation
 1 mL of EDTA requires = 20/V1 mg CaCO3 for complexation

This relation will be used in other two titrations

Titration-II: Estimation of total hardness of hard water sample

Pipette out 20 mL of the given sample of hard water into a clean conical flask. Add ~3 mL of
ammonia buffer (NH4OH – NH4Cl) solution and three drops of Eriochrome Black–T (EBT)
indicator. Titrate this mixture against standardized EDTA solution taken in the burette. The end
point is the change of color from wine red to steel blue. Repeat the titration for concordant titer
value. Let ‘V2’ be the volume of EDTA consumed.

S. Volume of sample hard water Burette reading (mL) Volume of EDTA

No. (mL) Initial Final (V2, mL)

1
2
3

Concordant titer value

9
Calculation:
From Titration 1, we have the following relation:
 1 mL of EDTA requires = 20/V1 mg CaCO3 for complexation
From Titration 2,
20 mL of sample hard water consumes = V2 mL of EDTA.
= V2 x 20/V1 mg of CaCO3 eq.
1000 mL of hard water sample consumes = V2 x 20/V1 × 1000/20
= V2/V1 × 1000 ppm
Total hardness of the water sample = “X” ppm

Titration-3: Removal of hardness using ion exchange method

Assemble the ion exchange column on to a burette stand and place a clean funnel on top of the
column. Pour the hard water sample (around 40 to 50 mL) remaining after the completion of
Titration – 2 through the funnel and into the ion exchange column. Place a clean beaker under the
column and collect the water passing through the column over a period of 10 minutes. Adjust the
valve of the column to match the duration of outflow.
From the water collected through the column, pipette out 20 mL into a clean conical flask and
repeat the EDTA titration as carried out above. Note down the volume of EDTA consumed as
‘V3’.

Calculations:
From Titration 1, we have the following relation:
 1 mL of EDTA requires = 20/V1 mg CaCO3 for complexation
From this relation, it can be seen that

20 mL of water sample after softening through the column consumes = V 3 mL of EDTA.

= V3 x 20/V1 mg of CaCO3 eq.
∴ 1000 mL of water sample after softening through the column consumes =
= V3 x 20/V1×1000/20
= V3/V1×1000 ppm
Residual hardness of the water sample = “Y” ppm

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 Volume of sample hard water Burette reading (mL) Volume of EDTA
S. No.
(mL) Initial Final (V2, mL)
1
2
3
Concordant titer value

Results:
1. Total hardness of the water sample = “X” ppm
2. Residual hardness in the water sample = “Y” ppm
3. Hardness removed through the column = X – Y ppm

Evaluation of Result:
Sample number Experimental Actual Value Percentage of Marks
value error awarded

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Experiment: 02 Date:

Water Quality Monitoring: Total Dissolved Oxygen Assessment in Different

Water Samples by Winkler’s Method
1. Importance of Dissolved Oxygen (DO): Knowledge of DO concentration in sea water is
often necessary in environmental and marine sciences. It is used by oceanographers to study
water masses in the ocean. It provides the marine biologist a means to measure primary
production, particularly in laboratory cultures. For the marine chemist, it provides a measure of
the redox potential of the water column. DO is also an important factor in corrosion. Oxygen is
poorly soluble in water. The solubility of oxygen decreases with increase in concentration of the
salt and hence, solubility of DO is lesser in saline water. The amount of DO at 100 % saturation
at sea level is 9.03 mg/L (at 20° C) and is sufficient to sustain aquatic life. Dissolved oxygen is
usually determined by Winkler’s method.

2. What is Winkler Method? The Winkler Method is a technique used to measure dissolved
oxygen in freshwater systems. DO is used as an indicator of the water body’s health, where
higher DO concentrations are correlated with high productivity and little pollution. This test is
performed on-site, as delays between sample collections and testing may result in an alteration in
oxygen content.

3. How does the Winkler Method Work? Winkler method uses titration to determine dissolved
oxygen in the water sample. A sample bottle is filled completely with water (no air is left to
skew the results). DO in the sample is then "fixed" by adding a series of reagents that form an
acid compound that is then titrated with a neutralizing compound that results in a colour change.
The point of colour change is called the "endpoint," which coincides with the dissolved oxygen
concentration in the sample. DO analysis is best done in the field, as the sample will be less
altered by atmospheric equilibration.

4. Applications:
Dissolved oxygen analysis can be used to determine the health or cleanliness of a lake or stream,
amount and type of biomass a freshwater, the amount of DO that a system can support and the
amount of decomposition occurring in the lake or stream.

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 Water Quality Monitoring: Total Dissolved Oxygen Assessment in
Experiment
Different Water Samples by Winkler’s Method
Dissolved oxygen (DO) is essential to living organisms in water but
Problem definition harmful if present in boiler feed water leading to boiler corrosion.
Methodology DO in water can be assessed using Winkler’s titration method.
Solution Estimation of total dissolved oxygen in different water samples.
Students will learn to
Student learning
a) perform Winkler’s titration method
outcomes
b) assess the total dissolved oxygen in different water samples

Principle: Estimation of dissolved oxygen (DO) in water is useful for studying the effect of
corrosion in boiler feed water and also for analyzing water pollution. DO is usually determined
by Winkler’s method. It is based on the fact that DO oxidize potassium iodide (KI) to iodine.
The liberated iodine is titrated against standard sodium thiosulphate solution using starch as
indicator. Since DO in water is in molecular state, as such it cannot oxidize KI. Hence,
manganese hydroxide is used as an oxygen carrier to bring about the reaction between KI and
Oxygen. Manganese hydroxide, in turn, is obtained by the action of NaOH on MnSO 4.

The liberated iodine (I2) is titrated against standard sodium thiosulphate (Na2S2O3) solution using
starch as indicator.

Requirements:
Reagents and solutions: Standard buffer of pH 7, standard KCl solution (0.01 M), standard
potassium dichromate (0.01 N), sodium thiosulphate solution, potassium iodide solution, alkali
Iodide solution (KI + NaOH in water), conc. H2SO4, manganese sulphate, starch solution as
indicator.

Apparatus: Conical flask, Burette, Measuring flask, Beakers.

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Procedure:
Titration 1: Standardization of Sodium Thiosulphate
The burette is washed and rinsed with sodium thiosulphate solution. Then the burette is filled
with given sodium thiosulphate solution. 20 mL of 0.01N K2Cr2O7 solution is pipetted out into a
clean conical flask. To this, add 5 mL of H2SO4 and 10 mL of 10 % KI. This is titrated against
sodium thiosulphate solution, when the solution become straw yellow in color, starch indicator is
added and the titration is continued further. The disappearance of bluish brown color indicates
the end point. The titration is repeated for concordant values.

Titration 2: Estimation of Dissolved Oxygen

100 mL of water sample is taken in a conical flask. 2 mL of MnSO 4 and 2 mL of alkali iodide
solution are added and shaken well for the rough mixing of the reagents. The flask is left aside
for few minutes to allow the precipitate to settle down and then add conc. H2SO4 dropwise until
the precipitate dissolves completely. It is further titrated against standard sodium thiosulphate
solution. When the solution turns straw yellow in color, add starch indicator. The end point is the
disappearance of bluish brown color. The titration is repeated for concordant values. From the
titer value, the strength of dissolved oxygen is calculated. Based on that, the amount of dissolved
oxygen in the water sample is calculated.

OBSERVATION AND CALCULATIONS

Titration - I: Standardization of Sodium Thiosulphate
Burette reading (mL)
Volume of K2Cr2O7 Volume of sodium
S. No.
(mL) Initial Final thiosulphate (mL)

Concordant value

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Calculations:
Volume of potassium dichromate V1 = 20 mL
Strength of potassium dichromate N1 = 0.01 N
Volume of sodium thiosulphate V2 =…………….mL (From Titration – 1)
Strength of sodium thiosulphate N2 = ……?
V1N1 = V2N2
 N2 = V1N1/V2
Strength of sodium thiosulphate = N2 = 20 × 0.01/V2 =…………….. N

Titration – II: Estimation of dissolved oxygen

Volume of water Burette reading (mL) Volume of sodium
S. No.
sample (mL) Initial Final thiosulphate (mL)
1
2
3
Concordant value
Calculations:
Volume of sodium thiosulphate V2 = ……… mL
Strength of sodium thiosulphate N2 = ………… N (From Titration – 1 calculation)
Volume of water sample taken V1= 100 mL
Strength of given water sample N1 = ?
V1N1 = V2N2
N1 = V2 X N2/100
= ……………. N
Amount of dissolved oxygen (ppm) = normality × equivalent weight of O2 × 1000 mg/L of the
given water sample.
= ……………….N × 8 g/L
= ……………….N × 8 × 1000 mg/L
= ------------------ ppm.

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Result: Amount of dissolved oxygen in the given water sample = ……… ppm.

Evaluation of Result:
Sample number Experimental Actual Value Percentage of Marks
value error awarded

16
Experiment: 03 Date:

Construction and working of an electrochemical cell

Principle: The electromotive force (emf) of an electrochemical cell is measured by means of a
potentiometer. An electrochemical cell (E cell) is considered as a combination of two individual
single electrodes. The potential difference between the two single electrode potentials is a
measure of emf of the cell (Ecell). In order to measure the potential difference between electrodes
in contact with electrolyte containing the same cation, it is necessary to have another electrode in
contact with electrolyte of same cation, both the half-cells connected through a salt bridge.
Saturated calomel electrode (SCE; E calomel) whose potential is known, is used as a reference
electrode and it is coupled with the metal electrode for which the potential is to be determined.

Hg / Hg2Cl2 (s), saturated KCl ║ (N/10) electrolyte of the metal / Metal

From the emf of the cell involving saturated calomel electrode and metal electrode dipped in its
solution of 0.1 N electrolyte, electrode potential of the metal electrode is readily calculated using
the standard potential of calomel electrode as;
Ecell = EM/M+ – Ecalomel
EM/M+ = Ecell + Ecalomel
Ecell is the total emf of the cell. The electrode potential of the metal electrode is given by Nernst
equation as;
EM/M+ = E° + RT In aMn+
nF
E°M/M+= EM/M+ - RT In aMn+
nF
E M/M = EM/M – 0.0595 log aMn+
° + +

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Table 1: EMF measured for various concentrations of M/M n+ system

Electrode/ Concentration of Ecell (V) EM/M+ = Ecell + E°M/M+= EM/M+ – 0.0595 log aMn+
Electrolyte Electrolyte (N) (EMF) Ecalomel n

0.01 N
2+
Zn/Zn 0.05 N
0.1 N
0.01 N
Cu/Cu2+ 0.05 N
0.1 N

Table 2: Individual activity coefficients of Cu2+ and Zn2+ in water at 25°C

Metal ion system

0.001 0.002 0.005 0.01 0.02 0.05 0.1 0.2
(Cu2+/Zn2+)

Activity coefficient (γc) 0.905 0.870 0.809 0.749 0.675 0.570 0.485 0.405

°
Solution Temperature (T) = C
The potential of saturated calomel electrode (SCE) = 0.244 + 0.0007 (25°C)

E°M/M+ = EM/M+ – 0.0595 Iog [γc x C] - - - - - - 1

n
where E ° is the standard electrode potential of the metal electrode; a Mn+ is the activity of metal
ions in the solution (aMn+ = γc[C]); γc is the activity coefficient (Table 2) and C is the
concentration of the electrolyte solution.
Requirements:
Reagents and solutions: Copper sulphate stock solution (0.1N), zinc sulphate stock solution
(0.1N), KCl salt.
Apparatus: Digital potentiometer, copper electrode, zinc electrode, calomel electrode, 100 mL
beaker, burette, standard flask.

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Procedure:
Calibrate the digital potentiometer with the help of the wires to display 1.018 V. The metal
electrode is sensitized by dipping in a small quantity of 1:1 nitric acid containing a small quantity
of sodium nitrite until effervescence occurs. Then the electrode is washed well with distilled
water. 50 mL of the given concentration of the electrolyte solution is taken in a beaker and its
corresponding metal electrode is introduced. This is connected with the saturated calomel
electrode (half-cell) by means of a salt bridge. The metal electrode is connected to the positive
terminal of and the calomel electrode is connected to the negative terminal of the potentiometer.
The emf of the cell (Ecell) is measured and noted in Table 1. The standard electrode potential
[E°M/M2+] is computed using Nernst equation (eqn. no. 1).

Construction of Daniel cell and measurement of its voltage with three different
concentrations of Copper and Zinc Solutions:

Fig.1. Daniel cell

In the Daniel cell, copper and zinc electrodes are immersed in the equimolar solution of
copper(II)sulfate and zinc(II)sulfate respectively. At the anode, zinc is oxidized as per the
following half-reaction:
Zn(s) → Zn2+(aq) + 2e−
At the cathode, copper is reduced as per the following reaction:
Cu2+(aq) + 2e− → Cu(s)
The overall reaction is:

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 Zn(s) + Cu2+(aq) → Zn2+(aq) + Cu(s)
Construct Daniel cell using the following concentrations of Copper and Zinc solutions and
record the voltage of the cells and enter into the Table 3.
Table 3: EMF of Daniel Cell observed from three different concentrations of zinc and
copper solutions

Metal Concentration Metal Concentration EMF observed

(N) (N) (Ecell / V)
0.01 N 0.01 N

Zn/Zn2+ 0.05 N Cu/Cu2+ 0.05 N

0.1 N 0.1 N

Result:
(a) The single electrode potential of zinc and copper systems are ___________ and
______________ respectively.
(b) Potentials (V) of Daniel cell: __________________

Evaluation of result:

Experimental Percentage of Marks

Sample No. Actual Value
Value error awarded

20
Experiment: 04 Date:

Material Analysis: Quantitative colorimetric determination of Ni2+ metal ions

using conventional and smart phone digital-imaging methods

1. Importance of the experiment: Nickel is a transition element and commonly exists in +2

oxidation state, though +1, +3 and +4 states are also observed in Nickel complexes. Nickel plays
an important role in biological systems as a constituent of several enzymes. Ni is also present in
soils and plants, and its concentration varies widely from trace quantities to being a major
constituent. Therefore, determination of nickel at different concentration levels in variety of
samples becomes very important.

2. Nickel Toxicity: Compared with other transition metals, Nickel is a moderately toxic element.
However, it is known that inhalation of nickel and its compounds can lead to serious problems,
including cancer in the respiratory system. Moreover, Nickel can cause a skin disorder known as
nickel-eczema (10.1016/j.kijoms.2016.08.003).

3. Nickel in Industries: A thin layer of nickel onto a metal object can be decorative, provide
corrosion resistance, wear resistance, or used to build up worn or undersized parts for salvage
purposes. Nickel alloys are used extensively because of their corrosion resistance, high
temperature strength and special magnetic and thermal expansion properties.
The major alloy types that are used are:
 Iron-Nickel-Chromium alloys
 Stainless Steels
 Copper-Nickel alloys and Nickel-Copper alloys
 Nickel-Chromium Alloys
 Nickel-Chromium-Iron alloys
 Low Expansion Alloys
 Magnetic Alloys (http://www.nickel-alloys.net/nickelalloys.html)

21
 Material Analysis: Nickel in Nickel-plated Component by
Experiment
Colorimetry
Corrosion protection in steel depends on the amount of Ni (acts as
Problem definition passivating metal) in its composition. Hence, it is important to analyze the
amount of Ni in steel for its use in industry.
Ni-DMG forms a stable colored complex, and its intensity depends on the
Methodology concentration of Ni present in solution. Colorimetric method is used to
measure the absorbance of the colored complex solution.
Estimation of Ni concentration in the unknown sample from the
Solution
calibration graph plotted based on different known Ni concentrations.
Students will learn to
Student learning
a) perform colorimetric method
outcomes
b) analyze the composition of Ni in different grades of steel

Principle: Dimethylglyoxime (DMG) reacts with nickel ions and forms a pink-colored
Ni(DMG)2 complex in alkaline medium. It gets oxidized by potassium ferricyanide
(K3[Fe(CN)6]) in alkaline medium to form a brown-red, water soluble oxidized Ni(DMG)2
complex as shown in the Scheme 1. Absorption spectrum of the oxidized complex shows
absorption maxima at a wavelength of 440 nm (Fig. 1). Concentration of Ni in the given
unknown sample is determined from the calibration graph as shown in Fig. 2.

Requirements:
Reagents and solutions: NiSO4 (1000 ppm), NaOH (1 N) solution, DMG (2 % in 2 N NaOH),
K3[Fe(CN)6] (1.5 %).
Apparatus: Colorimetry, Volumetric flasks, Beakers.

Procedure: Take 6 standard 50 mL volumetric flasks (including the unknown). To every flask
add 0.5 mL of DMG solution followed by 0.5 mL of K3[Fe(CN)6] solution using a burette.
Further, add 0.5, 1, 1.5, 2 and 2.5 mL of the working Ni stock solution (1000 ppm) from a
burette to get 10, 20, 30, 40 and 50 ppm of steel containing nickel(II) solutions. All the flasks are
shaken well and made up to 50 mL mark with 1N NaOH solution. Allow the flasks at least 15
minutes after adding all the reagents for the complete complex formation. Then the absorbance
of the formed brown-red solution is measured at 440 nm against distilled water (blank). Record
these absorbance readings in Table 1. Draw a calibration graph taking concentration of Ni2+ (in
ppm) as X-axis and absorbance readings as Y-axis. A straight line that passes through the origin

22
(see Fig. 2) is an indication that the measured data obeys Beer’s Law. From the calibration plot,
measure the concentration of nickel in the given unknown sample.

Scheme - 1

A
b
s
o
r
b
a
n
c Wavelength
e λ (nm)
Fig. 1: Absorption spectrum of oxidized Ni(II)- Fig. 2: Model calibration curve for
DMG complex showing λmax at 440 nm Ni(II) determination

Table 1: Experimental Data:

S. No. Concentration (ppm) (X-axis) Absorbance (Y-axis)

1.
2.
3.
4.
5.
6. Unknown

23
Using Mobile Application
The prepared standard solutions are lined up along with the blank and unknown concentration
sample. Take a photograph of each sample under the background white paper by holding the
camera about 50 cm away. The calibration curve will be constructed through the RGB values of
analytical response with different concentration of Ni2+ ions using smartphone app (RGB colour
detector). In the plotted graph, RGB response varies linearly vs the concentration of analyte. In
order to get precise analysis, follow
RGBtheMethod
steps givenFlow
below:
Chart

Transfer prepared standard solution and unknown solution

into different colorimetric test tubes

Take image of all test tube solution

using smart phone camera

Open the image processing app (RGB colour detector)

Go to gallery, open the image stored in app and

extract RGB values for each image/conc.

Process the RGB values (R/G) or (R/B) or (G/B)

etc., till to get linear response

Plot the calibration curve using RGB linear

response vs concentration

Find the unknown conc using the

calibration curve

24
Table 2: Extracted values of RGB response
Concentration RGB response
(ppm) R G B R/G R/B G/R G/B B/R B/G
0
1
2
3
4
5
Unknown

Result: Concentration of nickel in the given sample, as estimated by

(i) Conventional method = _________ ppm (mg/L)
(ii) Mobile application = ___________________ppm (mg/L)

Evaluation of Result:
Sample Percentage of Marks
Experimental value Actual Value
number error awarded

25
Experiment: 05 Date:

Polymer Characterization: Determination of viscosity-average molecular

weight of different natural/synthetic polymers by Viscometry

1. Importance of the experiment: Molecular weight of a polymer can be determined by

different techniques such as GPC, MALDI-TOF MS, etc. Determination of polymer molecular
weight through intrinsic viscosity using Ostwald viscometer is an absolute technique and is also
a cost-effective method. Viscosity is the measure of resistance offered to the flow of a solution.
Water has a viscosity of 1 cps (centipoise) at 25 oC and is considered as a standard.

2. Concept: Molecular weight of polymer (M) can be derived from intrinsic viscosity data of a
polymer solution. But one pre-requirement to determine the molecular weight of a polymer is the
knowledge of Mark-Houwink (M-H) coefficients. Upon substitution of intrinsic viscosity and
these coefficients in M-H equation, the molecular weight of the polymer can also be calculated.
M-H equation  = KMv, where K and  are M-H coefficients and  = intrinsic viscosity of
the polymer solution. In this experiment, we focus on the determination of intrinsic viscosity of
the given polymer solution. For a PVA solution at 25 ºC, the following values apply: K = 5.43 ×
10–4 and α = 0.64 (Kurata et al. 1975). In this experiment, we focus on the determination of
intrinsic viscosity of the given polymer solution as well as the concentration of given unknown
polymer solution.

3. Applications: Nowadays, polymers have become essential requirements in our day to day
activities. The end applications of the polymer depend upon its characteristics such as molecular
weight, polydispersity index, thermal stability, crystalline/amorphous nature, stereochemistry,
etc. Among these, molecular weight of the polymer is very important. LDPE (low density
polyethylene) is used as packing materials and carry bags, whereas UHMWPE (ultra-high
molecular weight polyethylene) is used as containers, tubing and other heavy-duty equipments
due to its high abrasion resistance, high impact strength and low coefficient of friction. Most of
the bottles for carbonated drinks, mineral water, edible oil and personal care products are made
of poly(ethylene terephthalate), PET and their intrinsic viscosity values range from 0.7-0.85
dL/g, depending on the length of the polymer chain (the longer the polymer chains, the more
entanglements between the chains and therefore the higher the viscosity).

26
Fig. 1: A portion of Ostwald viscometer Fig. 2: A plot of reduced viscosity vs.
showing the upper and lower graduation concentration of a polymer solution, y-intercept
marks, 'a' and 'b' respectively. corresponding to intrinsic viscosity.

Viscosity is the measure of resistance of a fluid to flow. Longer the polymer

chains, the more entanglements between the chains and therefore the higher the
Problem definition
viscosity. Molecular weight of polymer (M) can be derived from intrinsic
viscosity data of a polymer solution.
Determination of intrinsic viscosity using Ostwald viscometer. In a particular
Methodology solvent, concentration of the polymer is directly proportional to viscosity of the
solution.
Determination of intrinsic viscosity of the given polymer sample and the
Solution
concentration of given unknown polymer sample.
Students will learn to
Student learning
a) Determine intrinsic viscosity of the given polymer solution
outcomes
b) Estimate the unknown polymer solution concentration

Principle: When a polymer is mixed with a solvent, the solvent enters into the polymer matrix
and swelling of polymer coils takes place. This expanded polymer
coil disintegrates and moves out of polymer matrix and dissolves
in the solvent. The apparent volume occupied by the expanded
coil is referred to as the `hydrodynamic volume’ of the polymer
molecule in the solution under flow. Viscosity of a polymer
solution is a direct measure of hydrodynamic volume of the
polymer, which in turn, is a measure of its molecular weight.
Viscosity of a polymer is more in a good solvent than in a poor
solvent.

Reagents: PVA (polyethylene glycol) solution of different concentrations, Distilled water.

27
Apparatus: Ostwald viscometer, stop-clock, 50 mL standard flasks

Procedure: Prepare at least 4 different diluted concentrations of PVA (0.1 to1.0%) in water
using 1 % PVA stock solution (1 g/100 mL). Initially, rinse the Ostwald viscometer with a little
amount of water. Fill it with 20 mL pure water and use a rubber filler to suck the water above the
upper mark. By keeping the upper mark of the small reservoir of viscometer parallel to eyes,
allow the solvent to flow down to the lower mark and note down time in seconds. This is known
as the Eflux time. Repeat the same experiment for 3 times to get the average E flux time for water
(t0). Apply the same procedure to determine the flow rate for remaining 3 diluted solutions as
well as the given unknown concentration of PEG and note down their flow time in seconds.
Calculate relative viscosity, specific viscosity and reduced viscosity as shown in the Table 1.
Plot the graph between polymer concentrations (C g/mL) vs sp/C (red). The value of intercept at
C = 0 will give intrinsic viscosity of the polymer solution (see Fig. 3). Also, from the red value
of the unknown sample, its concentration is also estimated as shown in Fig. 3.

Table 1: Viscosity measurement data

Eflux time for pure water (t0) = _______sec.

Eflux time, t (sec)

Concentration,
S. No. r = ts/t0 sp = r-1 red = sp/c
C (g/mL)
t1 t2 t3

28
 Fig. 3: Concentration (C, g/mL) Vs sp/C

Using the value of intrinsic viscosity from the graph and the M-H coefficients, the molecular
weight of the polymer can also be calculated. M-H equation  = KMv, where K and  are M-
H coefficients and  = intrinsic viscosity of the polymer solution.

Result:
Molecular weight of the given polymer in Daltons (M) =

Evaluation of Result:
Experimental Percentage of
Sample number Actual Value Marks awarded
value error

29
Experiment: 06 Date:

Estimation of Sulphate for Assessing Water Contamination by Conductivity

Method

Sulphate (SO42-) is found in almost all natural water. Origin of most sulphate compounds is the
oxidation of sulphite ores, presence of shales or the industrial wastes. Ground water moving
through soil and rocks containing sulphate minerals result in higher dissolved sulphate ions than
permissible limit.

Problems due to excess sulphate ion concentration in water:

 Sulphates cause scale formation in boilers, pipes, etc.
 High sulphate concentration will leads to corrosion on copper piping.
 Sulphate has a laxative effect and creates diarrhoea leading to dehydration in humans and
animals.
 High sulphate concentration leads to eutrophication of water bodies leads to reduction of
dissolved oxygen Sulphate will give bitter taste to water if the concentration exceeds
beyond 250 ppm.

Methods to estimate sulphate ion concentration in water:

1. Turbidimetric method: It involves the measurement of turbidity formed when an aliquot of
BaCl2-gelatin reagent is added to acidified sulphate solution.
2. Titrimetric method: By dissolving precipitated BaSO4 in excess of EDTA solution and the
excess EDTA is back titrated with standard Zinc solution.
3. Colorimetric Measurement: Based on the reaction of barium chloranilate with sulphate ion
at pH 4 in ethanol yield highly coloured acid-chloranilate ion and is measured at 530 nm.
4. Conductometric method: This method measures the conductivity of the solution as the
titration proceeds. Conductance tends to vary with the characteristics of the solvent, number,
size and charge of the ions involved. When one ion is replaced by another ion significantly
during the titration, conductance will change in a linear manner until the replacement is
complete. After that, the slope of the line changes due to the addition of another ion with
difference conductance.

30
Problem definition People using water with high levels of sulfate are vulnerable to
dehydration and diarrhea. Kids are more sensitive to sulfate than adults.
Methodology Conductivity of the soluble sulphate solution will change when it is
precipitated by BaCl2. Conductivity will reach minima when all sulphate
ions are precipitated, and from which, the total amount of sulphate ion
present in the water can be determined.
Solution Amount of BaCl2 required to remove the dissolved sulphate can be
estimated.
Student learning Students will learn to
outcomes a) perform conductometric method
b) remove sulphate ion from irrigate water

Principle: Electrolyte solutions conduct electricity due to the presence of ions in solution. In
case of precipitation titration between BaCl2 and Na2SO4, the conductance decreases slowly due
to the removal of SO42- from the solution upto the equivalence point. After the equivalence
point, the conductance increases rapidly due to the excess addition of Cl- as BaCl2 which remains
in solution as Ba2+ and Cl-. This makes detection of neutralization point easy from the
conductance trend plotted as a graph. This is the principle used in the estimation of SO 42- from
contaminated water sample.

Requirements:
Reagents and solutions: BaCl2 (0.02 M), Na2SO4 (0.01 M), unknown sulphate solution and
distilled water.

Apparatus: TDS-Conductivity Bridge, Conductivity cell, Burette, Pipette, Volumetric flasks,

Glass rod, Beaker (100 mL).

Procedure:
Calibration of TDS-Conductivity meter: Place a freshly prepared 0.01 M KCl solution (given
in bottle) in a 100 mL beaker. Dip the conductivity cell in this solution and connect to the TDS-
Conductivity meter. Press “CAL” button and complete the internal calibration of the instrument.

Standardization of BaCl2 (Titration – 1):

In a 50 mL standard flask, fill with solution upto the mark resulting in a solution containing 0.96
mg/mL of sulphate ions (Mol. wt. of SO42- = 96.06). Pipette out 20 mL of 0.01 M Na2SO4
solution from Bottle A into a 100 mL beaker and add ~20 mL of distilled water to it. The

31
conductivity cell is dipped into the beaker and connected to TDS conductivity meter. Fill the
burette with 0.02 M BaCl2 solution from Bottle B. Record the conductivity of the sulphate
solution as 0th reading. Add 1.0 mL BaCl2 of known concentration into the beaker, stir with glass
rod and note down the conductance. Continue the addition of BaCl2 (1.0 mL each time) and note
the conductance after each addition. Continue the titration beyond the equivalence point for
about 5 mL. The conductance will decrease till complete precipitation of BaSO 4 and then
increases as the addition of BaCl2 is continued. A graph is now drawn by plotting conductance vs
volume of BaCl2 added. Intersection point from the plot gives the volume of BaCl2 required for
precipitating the sulphate present in the known sample.

Estimation of unknown sulphate in the given solution (Titration – 2):

Make up the given unknown sulphate solution (sulphate ion contaminated water sample) in a
clean 50 mL standard flask. Pipette out 20 mL of this solution into a 100 mL beaker and add 20
mL distilled water to it. Dip the conductivity cell and repeat the above procedure with the
unknown sulphate solution and determine the amount of BaCl2 required for precipitating the
unknown sulphate in the sample.
From the two titrations carried out, calculate the amount of sulphate present in the effluent
sample.

32
Table 1: Conductometric Titrations
Titration-1: Standardization of BaCl2 Titration-2: Estimation of sulphate content
Burette: BaCl2 solution (0.02 M) Burette: std. BaCl2 solution
Beaker: 20 mL of Na2SO4 (0.01 M) + 20 Beaker: 20 mL of unknown sulphate solution +
mL of distilled water 20 mL of distilled water
Electrode: Conductivity cell Electrode: Conductivity cell

Volume of BaCl2 Conductance Volume of BaCl2 Conductance

added (mL) ( mhos) added (mL) ( mhos)
0.0 0.0
1.0 1.0
2.0 2.0
3.0 3.0
4.0 4.0
5.0 5.0
6.0 6.0
7.0 7.0
8.0 8.0
9.0 9.0
10.0 10.0
11.0 11.0
12.0 12.0
13.0 13.0

33
Fig 1: Model graphs - 1and 2 for TDS-Conductometric estimation of known and unknown
sulphate sample solutions, respectively.

Calculations:

A). Standardization of 0.02 M BaCl2:

(M1 x V1) of BaCl2 solution = (M2 x V2) of sodium sulphate

Molarity (M1) of BaCl2 solution = (0.01 M x 20 mL) / Volume measured from Plot-1 (V1)
= _______________ M

B). Estimation of unknown sulphate:

(M3 x V3) of irrigation water sample = (M1 x V1) of BaCl2 solution

Molarity of sulphate contaminated water sample = M1 of BaCl2 x Volume measured from Plot-2
(V3) /20 = ________________ M

Amount of sulphate present in 1L = Molarity (M3) of irrigation water sample x Mol. wt. of SO42-
(96.06)
Amount of sulphate present in given sample solution = Strength of irrigation water sample x
96.06 x 100 / 1000 = __________ grams in 100 mL

Result: Amount of sulphate in given irrigation water sample =_________ grams.

Evaluation of Result:
Sample number Experimental Actual Value Percentage of Marks
value error awarded

34
Experiment: 07 Date:

Material Analysis: Estimation of Iron in Carbon Steel by Potentiometry

1. Significance: Steel production is an index of national prosperity and economy, and is globally
used in variety of industrial sectors like ship building, automobiles, construction, machinery and
tools. Carbon steel is one variety in which nearly 96 % of iron is alloyed with nearly 2 % of
carbon and other elements like manganese, chromium, nickel and copper. The composition is
varied for achieving desired strength, ductility and long-term wearing-off properties. Thus,
qualitative determination of iron in steel is very important.

2. Concept: Potentiometric titration is a process of determining the quantity of a sample by

adding increased quantities of a titrant until the end-point. The potential difference between
indicator and reference electrodes is measured under conditions where the current passed is
sufficiently small to maintain thermodynamic equilibrium. Potentiometric titrations provide
reliable data than other conventional titrations with chemical indicators in particular with
coloured or turbid solutions. In this experiment, Fe 2+ is oxidised to Fe3+ by K2Cr2O7 as a redox
titration.
6Fe2+ + Cr2O72- + 14H+ → 6Fe3+ + 2Cr3+ + 7H2O
Change in the concentration of Fe2+ ions during the addition of K2Cr2O7 is monitored by
measuring the solution potential which forms the basis for this experiment. From Nernst
equation, a measurable quantity - voltage or potential is related to the concentration of species
(Fe3+/Fe2+) in the solution.
RT Fe 3
E  E0  ln( 2 )
nF Fe
At the end point, a rapid change in the potential would be observed indicative of the complete
conversion of Fe2+ to Fe3+. A plot of observed potential vs volume of K2Cr2O7 consumed or its
first derivative graph (E/V vs average volume of K2Cr2O7) is used to detect the titration end
point, which in turn, is used to qualitatively measure the amount of Fe 2+.

3. Applications: Potentiometric method is an electroanalytical technique which can be used to

determine accurately the iron content in steel samples for industrial applications without using

35
 Mechanical properties of steel depend on its composition. Hence, it is
Problem definition important to analyze the amount of Iron in steel for industrial
applications.
Potentiometric method using K2Cr2O7 (oxidizing agent) to oxidize Fe(II)
Methodology
in steel to Fe(III) facilitates the estimation of Iron in steel.
Solution Estimation of iron (%) in different steel samples.
Students will learn to
Student learning
a) perform potentiometric method
outcomes
b) analyze the composition of iron in different grades of steel
any indicator. This method is also useful for dilute or unknown samples or compositions for
which identification of appropriate chemical indicators are challenging.

Principle: Potassium dichromate (K2Cr2O7) oxidizes ferrous ion to ferric ion in the presence of
acid as per the reaction:
3Fe+2 → 3Fe+3 + 3e- .......(1)
Cr2O72- + H2O + 3e- → 2CrO42- + 2H+ .......(2)
Overall, 3Fe+2 + Cr2O72-+ H2O → 3Fe+3 + 2CrO42-+ 2H+
Electrode potential (oxidation potential) in the titration depends upon the concentration of Fe2+,
Fe3+ and H+ ions. To avoid the effect of the change in H+ ion concentration, the titration is
usually carried out in large excess of acid. Oxidation potential of this redox system is given by
RT Fe 3
E  E0  ln( 2 )
nF Fe
Connecting the redox electrode (Platinum) with a saturated calomel electrode (SCE) completes
the necessary cell as indicated below:
HgHg2Cl2 (s), Saturated KCl  Fe3+, Fe2+Pt
When K2Cr2O7 is added, Fe2+ is oxidized to Fe3+ whose concentration increases with progressive
addition of K2Cr2O7. The observed EMF gradually increases. At the end point, there will be a
sharp increase due to the sudden removal of all Fe 2+ ions. Plot-1: EMF measured (E) vs Volume
of K2Cr2O7 added and Plot-2: E/V vs Average volume of K2Cr2O7 was drawn. End point of
the titration is measured from the Plot-2 graph.

Requirements:

36
Reagents and solutions: K2Cr2O7 (0.05 N), Unknown steel solution, 2 N H2SO4.

Apparatus: Calomel electrode, Platinum electrode, Potentiometer, Volumetric flasks, Burette,

Pipette, Beakers.

Fig. 1: Typical apparatus for Fig. 2: Typical Potentiometric titration curves.

potentiometric titrations. (a) Normal curve and (b) First derivative curve.
Procedure:
Calibration of Potentiometer: Switch on the potentiometer and connect the standard cell
terminals to either channel A (move channel switch to position A) or channel B (move the
channel switch to position B). The meter should read 1.018 V. In case it is not 1.018 V, adjust
the std. knob to obtain reference value.

Estimation of Fe(II) in steel: Transfer the given unknown steel [containing Fe(II)] solution into
a clean 50 mL standard flask and make the solution up to the mark with distilled water and mix
well. Pipette out 20 mL made up steel sample solution into a clean 100 mL beaker and add one
test tube of dil. H2SO4 (2 N). Place Pt electrode in the beaker and connect to the positive terminal
of the potentiometer. In another beaker, place 50 mL of saturated KCl solution and dip the SCE
in the solution and connect to the negative terminal of the potentiometer. Connect the beakers
with a salt bridge to complete the cell. Read the EMF of the cell and note down the value. Add
1 mL of K2Cr2O7 solution from the burette to the beaker containing steel sample solution. Stir
the solution carefully and measure the EMF. Continue the addition of K2 Cr2O7 solution and
record the EMF for every 1 mL addition until the potential shows a tendency to increase rapidly.
Once the abrupt change in cell EMF is observed, continue the titration to take 5 more readings.
Plot EMF (ordinate) vs. volume of K2Cr2O7 added (abscissa) to get S-shaped curve which
indicate the volume range of the end point.

To find out the volume of end point more precisely, carry out the second titration in a similar
way but by adding 1 mL aliquots of K2Cr2O7 initially and then 0.1 mL aliquots between the two

37
volumes where the end point is detected. Continue the titration beyond the end point as done
above. The exact end point is determined by differential method i.e. by plotting ΔE/ΔV vs
average volume of K2Cr2O7 added. Calculate the normality of the Fe(II) in the given solution.

OBSERVATIONS AND CALCULATIONS

Potentiometric Titration-I:
Burette: K2Cr2O7 solution (0.05 N)
Beaker: 20 mL of steel solution containing Fe(II) + 20 mL (one test tube) of dil. H 2SO4
Electrodes: Indicator electrode (Pt) to red terminal and SCE to black terminal.
Volume of EMF Volume of EMF
S. No. S. No.
K2Cr2O7 (mL) (volts) K2Cr2O7 (mL) (volts)
1 11
2 12
3 13
4 14
5 15
6 16
7 17
8 18
9 19
10 20

Fig. 3: Plot of EMF vs Volume of K2Cr2O7 Fig. 4: Plot of ΔE/ΔV vs Average volume of
added (mL) K2Cr2O7 added.

38
Potentiometric Titration-II:
Burette: K2Cr2O7 solution (0.05 N)
Beaker: 20 mL of steel solution containing Fe(II) + 20 mL (one test tube) of dil. H 2SO4
Electrodes: Indicator electrode (Pt) to red terminal and SCE to black terminal

Sl. Vol. of K2Cr2O7 EMF E E/V Average

V (mL)
No. ( mL) (Volt) (Volt) (Volt/mL) Volume (mL)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22

39
Calculations:
(N x V) of steel sample solution = (N x V) of K2Cr2O7

N of steel sample solution = 0.05 N x Volume of K2Cr2O7 from Plot-2

20 mL of steel sample
= _____________N

Amount of Fe present in 1L of sample solution = Normality of steel sample x Atomic weight of Fe (55.85)
Amount of Fe present in given sample solution = Normality of steel sample x 55.85 x 100
1000
=________________grams in 100 mL

Result: The amount of Iron present in given steel sample is found to be =_________ grams.

Evaluation of Result:

Sample number Experimental Actual Value Percentage of Marks awarded

value error

40
Experiment: 08 Date:

Quantitative colorimetric determination of Fe2+ metal ions using conventional

and smart phone digital-imaging methods

Experiment Determination of ferrous iron in cement by colorimetric method

Corrosion protection in steel depends on the amount of Ni (acts as
Problem definition passivating metal) in its composition. Hence, it is important to analyze the
amount of Ni in steel for its use in industry.
Iron and 1,10- Phenanthroline forms a stable colored complex. With
Methodology increasing concentration of Fe2+ in solution, its color intensity also
increases. The intensity of the color can be measured using a colorimeter.
Estimation of Fe2+ concentration in the unknown sample from the
Solution
calibration graph plotted based on different known Fe2+ concentrations.
Students will learn to
Student learning
a) Perform colorimetric response analysis
outcomes
b) Quantitative determine of Fe2+ in different grades of cement.

Principle:
A complex of iron (II) is formed with 1,10-phenanthroline, Fe(C12H8N2)32+, and the absorbance
of this colored solution is measured with a spectrophotometer. The spectrum is plotted to
determine the absorption maximum. Hydroxylamine (as the hydrochloride salt to increase
solubility) is added to reduce any Fe3+ to Fe2+ and to maintain it in that state.

41
Requirements:
Reagents and solutions:
1) Standard iron (II) solution - Prepare a standard iron solution by weighing 0.0176g of
ferrous ammonium sulfate, (Fe(NH4)2(SO4)2.6H2O). Quantitatively transfer the weighed
sample to a 250mL volumetric flask and add sufficient water to dissolve the salt. Add 0.7mL
con. Sulphuric acid, dilute exactly to the mark with distilled water and mix thoroughly. This
solution contains 10mg iron per Liter (10 ppm).
2) 1,10-phenanthroline solution - Dissolve 25mg of 1,10-phenanthroline monohydrate in
25mL water. Store in a plastic bottle.
3) Hydroxylamine hydrochloride solution - Dissolve 10g of hydroxylamine hydrochloride in
100mL water.
4) Sodium acetate solution - Dissolve 10g of sodium acetate in 100mL water.

Apparatus: Colorimetry, Volumetric flasks, Beakers.

Procedure:
Into a series of 100mL volumetric flasks, add 1.00, 2.00, 5.00, 10.00 and 25.00 mL of the
standard iron solution with pipettes. Into another 100mL volumetric flask, place 50mL distilled
water for a blank. The unknown sample will be furnished in another 100mL volumetric flask.
To each of the flasks (including the unknown) add 1.0mL of the hydroxylammonium chloride
solution and 5.0mL of the 1,10-phenanthroline. The Iron (II)-phenanthroline complex forms at
pH 2 to 9.Add 5mL of sodium acetate to neutralize the acid present and adjust the pH to a value
at which complex forms. Dilute each solution to exactly 100mL. The standards will correspond
to 0.1, 0.2, 0.5, 1 and 2.5 ppm of iron, respectively. Allow at least 15 minutes after adding the
reagents before making absorbance measurements so that the color of the complex can fully
develop. Once developed, the color is stable for hours.
Obtain the absorption spectrum of 2.5-ppm solution by measuring the absorbance from about
400 to 700nm or the range of your instrument. The blank solution should be used as reference
solution. Plot the absorbance against the wavelength and select wavelength of absorption
maximum.

42
 Concentration Absorbance

Prepare a calibration curve by measuring the absorbance of each of standard solutions of

wavelength of maximum absorbance. Measure the unknown in the same way. Prepare a
calibration curve by plotting absorbance of standards against concentration in ppm. From this
plot and the unknown's absorbance, determine the final concentration of iron in your unknown
solution.

Using Mobile Application

The prepared standard solutions are lined up along with the blank and unknown concentration
sample. Take a photograph of each sample under the background white paper by holding the
camera about 50 cm away. The calibration curve will be constructed through the RGB values of
analytical response with different concentration of Ni2+ ions using smartphone app (RGB colour
detector). In the plotted graph, RGB response varies linearly vs the concentration of analyte. In
order to get precise analysis, follow the steps given below:

43
 RGB Method Flow Chart

Transfer prepared standard solution and unknown solution

into different colorimetric test tubes

Take image of all test tube solution

using smart phone camera

Open the image processing app (RGB colour detector)

Go to gallery, open the image stored in app and

extract RGB values for each image/conc.

Process the RGB values (R/G) or (R/B) or (G/B)

etc., till to get linear response

Plot the calibration curve using RGB linear

response vs concentration

Find the unknown conc using the

calibration curve

44
Table 1: Extracted values of RGB response

Concentration RGB response

(ppm) R G B R/G R/B G/R G/B B/R B/G
0
1
2
3
4
5
Unknown

Result: Concentration of nickel in the given sample, as estimated by

(i) Conventional method = _________ ppm (mg/L)
(ii) Mobile application = ___________________ppm (mg/L)

Evaluation of Result:
Sample Percentage of Marks
Experimental value Actual Value
number error awarded

45
Experiment: 09 Date:
Acid-base titration with Aurdino

Introduction:
Acid-base titration is a common lab experiment and finds its application is wide variety of
problems. Here in the proposed experiment, strong acid (HCl) is titrated against weak base
(Na2CO3) and change in pH is monitored using a pH meter. When the pH reaches 7, it indicates
the end point. This is the experiment done normally in the chemistry lab.
Instead of using a pH meter (as in the conventional experiment), the student will use Aurdino
board to acquire and process the data obtained from the pH probe. Aurdino is an open source
electronics board, finding its application in all the domains of science and technology. Aurdino
board is programmable and connected to the laptop to get the data. It can also be connected to
mobile to obtain the data by preinstalling the program in the Aurdino.
Experiment:
When acid is titrated with base, there will be change in pH of the resulting solution. The pH
probe will measure the pH and will give the output as voltage. This voltage is then feed in to the
Aurdino board as analog input and can be measured in the computer.

Fig. 1: Pictorial representation of the experimental setup

Motivation behind this experiment:

46
One of the drawback in our Indian system is that the student uses instruments as a black box
without having any idea of how the instruments works (including the electronics, data acquisition
and processing). As an engineering student, he should be fully aware of instrumentation. As a
first step to bring an engineering feeling among feeling students, we are introducing
instrumentation in chemistry curriculum where the students learns chemistry through electronics.
From these kinds of experiments in first semester, students get strong motivation and develops
interest in instrumentation who at the later stage can build instruments of his own. By this we
make the student to discover the engineer within himself.
Course outcome:
After the end of this experiment, the students can
1) Learn chemistry behind acid acid-base titration.
2) Measures pH of any solution
3) Can use and program Aurdino board and apply it to measure and control any other
property or devices respectively.
4) Acquire the knowledge of data acquisition and electronics.
5) Understand the technology behind the measurement and instrumentation.
6) Since the Aurdino is programmable, the student has flexibility to alter the experiment and
can play with it.

Real setup with pH probe and Aurdino: [Ref: https://www.sparkyswidgets.com/portfolio-

item/ph-probe-interface/ ]

47
48
Physical connections
Step 1: Connect 5 V in the UNO board to the Vcc of the signal conversion board.

Step 2: Connect ground (GND) in the UNO board to the ground in the signal conversion board

Step 3: Connect P0 in the signal conversion board to the A0 (analog input) in the UNO board

Step 4: Connect UNO and the computer through the USB cable.

Step 5: Prepare known solution of different pH for calibration of signal conversion board

Step 6: The measured voltage is between 0-5 V and arduino shows this as an integer between
0 – 1023 (i.e 0 corresponds to 0 V and 1023 corresponds to 5 V, resolution =5 V/1023)

Step 7: Measure the number given by the Arduino for solution with different concentration.
(knobs are given in the signal conversion board to adjust the resistance for easy calibration

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and the conversion can be incorporated in the code itself).

Step 8: Now setup is ready for measurement. Unknown solution of any pH can be measured.
With this, acid-base titration can be performed.

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