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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).

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 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.
Hardness of Water
1

Dissolved Oxygen
2

Electrochemical Cell
3

Colorimetric determination of Ni2+

4

Viscosity
5

Estimation of Sulphate by Conductometry

6

Estimation of Iron in Carbon Steel by

7 Potentiometry

Colorimetric determination of Fe2+

8

Student signature Faculty Signature

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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

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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+

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cations in hard water are exchanged with Na+ or H+ ions in the resins. It is followed by passing
through anion-exchange resins packed column for the removal of HCO3-. CO32-, Cl-/SO42-/NO3-
The exhausted resins can be regenerated by passing brine solution or 10 % dil. HCl or
KOH/NaOH 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 CaCO3 (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 ‘V1’ 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 20 0 20.4 20.4

2 20 0 20.2 20.2

3 20 0 20.2 20.2

Concordant titer value 20.2

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 20 0 8.1 8.1
2 20 0 7.8 7.8
3 20 0 7.8 7.8

Concordant titer value 7.8

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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 = V3 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 20 0 0.3 0.3
2 20 0 0.3 0.3
3 20 0 0.3 0.3

Concordant titer value 0.3

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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