Department of Robotics and Mechatronics Engineering

University of Dhaka
Course No. RME 1115 (Chemistry Loboratory)
Chemistry Laboratory Manual

Books Recommended:

A Text Book of Macro and Semi-micro Qualitative Inorganic Analysis, A. I. Vogel, 4 th edition,
Longmans
Vogel’s Textbook of Quantitative Inorganic Analysis, 3rd/4th edition, ELBS/Longmans
Vogel’s Textbook of Practical Organic Chemistry, 5th edition, Longmans
Practical Physical Chemistry by A. Faraday

Centrifugate

/ Residue

This lab is a 1.5 credits course with 30 hours duration and carries 100 marks. 40% of the total
marks are taken as the continuous assessment, 40% of the total marks are allotted for final
examination, 15% for viva voce and 5% for attendance. The continuous assessment of this
course is made through students’ performance at work, viva voce (or presentation), and
evaluation of practical reports. Final examination will be held after finishing the written
examinations of theoretical courses.
In this lab, students are supposed to work in groups; a group usually comprises three (or four)
members.
Safety in the Laboratory

The Cardinal Rule for Safety in the Laboratory:

Work cleanly and deliberately; don’t rush; above all, think before you act.

The following rules have been drawn up to assist in protecting you and others when you are
working in laboratories of the Department of Robotics and Mechatronics Engineering at Dhaka
University. They, in no way, form a complete and absolute statement to cover all situations that
you may encounter in your laboratory work; rather, they are designed to cover most common
situations.

(i) Keep your working area free of mobiles, purses, excess chemicals, equipment and trash. All
spills must be cleaned up immediately and the floor around you must be kept dry. Your work
space must be left clean and neat at the end of each laboratory period. You are responsible for
cleaning all sinks and apparatus you have been working with. Any borrowed equipment must be
returned to its proper storage place in the laboratory.

(ii) Wear a lab coat at all times when you are in the laboratory to protect your clothes and skin
from chemicals.

(ii) Wear eye protective glasses at all times when you are in the laboratory. Do not forget that
eyes are one part of your body that often cannot heal themselves from an injury.

(iii) Do not place anything in your mouth while you are in the lab: no food, no finger-nails, no
ball-point pen, no smoke, nothing. The hazards of accidentally ingesting dangerous substances
while doing this are obvious. Carefully wash your hands after you have finished your lab work.

(iv) Do not make practical joking, pushing, running, ‘horse play’ in any laboratory. Use your
common sense and good judgment. Good laboratory work can be a fun and rewarding, but
laboratories are dangerous places to play in.

(v) No unscheduled experiments until permission have been granted for that experiment.
Provided the experiment is safe and relevant to your study, permission will normally be granted.

(vi) Seek your teacher’s permission if you need more work to do in any laboratory in addition to
your regularly scheduled times. Never work alone in any laboratory.

(vii) Never use unauthorized chemicals as substitutes in an experiment without getting specific
permission from your teacher.

(vii) If you get any chemicals in your eye, mouth, or any parts of your body that can cause severe
irritation or damage to the sensitive tissue of your body, wash with water immediately until the
irritation is cleared, and make sure that the incident is reported to your teacher.
 Dept. of Robotics & Mechatronics Engineering
Course name: Chemistry Lab (1.5 Credit)
Course Code: RME 1115

Experiment No: 1

Name of the experiment: Standardization of NaOH Solution with a standard oxalic acid solution.

Principle: Titration is a process of determining the volume or strength of an acid or base by

adding it to base or acid of known volume and concentration. NaOH is a secondary standard
strong base and (COOH)2.2H2O is a primary standard acid.

Objective: To standardize a basic solution by volumetric analysis (Titration).

Equipment/Apparatus: Burette, Pipette, Volumetric flask, Conical flask.

Chemicals: і) NaOH
іі) Oxalic acid [(COOH)2.2H2O]
ііі) Phenolphthalein indicator solution

Preparation of standard 0.05M Oxalic acid: About 0.63g of crystalline Oxalic acid dihydrate
[(COOH)2.2H2O] is measured out in an electric balance. Dissolve it in a 100 mL volumetric flask
with little amount of distilled water and fill it up to the mark.

Working Procedure:
і) Take the supplied sodium hydroxide solution in the burette.
ii) Pipette out 10.0 mL of the prepared oxalic acid into a conical flask.
ііі) Add 1 or 2 drops of Phenolphthalein indicator.
iv) Record the initial burette reading
v) Add NaOH solution from the burette into the conical flask with constant shaking until the
colour changes and record the final burette reading.
vi) Repeat the procedures (ii-iv) at least three times and take the average.
vii) Calculate the concentration in terms of Molarity.
Titration Table:

Observation Volume of Burette Reading (mL) Vol. of Average

No. (COOH)2.2H2O NaOH (mL) volume of
(mL) Initial Final NaOH (mL)

1
2
3

Reaction:

a HOOC-COOH (aq) + b NaOH (aq) → p NaOOC-COONa (aq) + q H2O (l)

Calculation:

We know that,

S1V1 S2V2
Where,
a = b
S1 = Strength of oxalic acid
V1 = Volume of oxalic acid
S2 = Strength of NaOH
V2 = Volume of NaOH
 Dept. of Robotics & Mechatronics Engineering
Course name: Chemistry Lab (1.5 Credit)
Course Code: RME 1115

Experiment No. 2

Name of the experiment: Standardization of a given HCl solution with standard Na 2CO3
solution.

Introduction: The experiment comprises basically volumetric determination based on reactions of

acids with alkalis, i.e. neutralization of acids and bases:
H+(aq) + OH ‾(aq) → H2O(l)

Hydrochloric acid is a secondary standard substance, as its concentration varies due to its fuming
action and hence its standard solution cannot be prepared directly. On the other hand, the
primary standard Na2CO3 is a crystalline substance, stable at atmospheric conditions and
corresponds exactly to its formula, which can be obtained chemically pure. Thus Na 2CO3 can be
used to prepare a standard solution and with it standardize the hydrochloric acid.

Preparation of a standard sodium carbonate solution (0.1 M)

Procedure: Weigh out accurately about 1.0599 g pure anhydrous Na 2CO3 and then transfer it to a
100 mL volumetric flask. Dissolve it in distilled water by shaking well and make the solution up
to the mark of the volumetric flask.

Standardization of the supplied hydrochloric acid solution by the standard sodium carbonate
solution

Procedure: Pipette out 10 mL of the standard sodium carbonate solution and transfer it into a
conical flask and dilute this to about 50 mL with distilled water and then add few drops of
methyl orange indicator. Now titrate the solution with supplied hydrochloric acid from a burette.
During the addition of the acid the conical flask must be rotated constantly and continue the
addition of the acid until the colour of
the solution becomes very faint yellow.
Wash the walls of the flask with little
distilled water and continue the titration
very carefully by adding the acid drop
wise until the colour becomes orange or
faint pink. Repeat the titration for
two/three times. Record your burette
reading to two decimal places. The
titrations should agree within 0.1 mL.
Calculate the concentration of the
supplied sodium carbonate solution.
Titration technique
Sodium carbonate reacts with hydrochloric acid according to the following equation:

Na2CO3(aq) + 2HCl(aq)  2NaCl(aq) + H2O(l) + CO2(g)

Calculation:
Where,

S1V1 = S2V2 S1 = Strength of Na2CO3

V1 = Volume of Na2CO3
S1  V1 S2 = Strength of HCl
S2 = V2 = Volume of HCl
V2

Experiment No. 3
Name of the Experiment: Standardization of a given thiosulphate solution with standard
K2Cr2O7 solution.

Introduction: Quantitative determination dealing with the titration of iodine liberated in

chemical reactions is called iodometry whereas iodimetry refers to the titrations using standard
iodine solution. The following redox reactions are involved in this experiment:

6I-(aq) + Cr2O7 2-(aq) + 14 H+(aq)  3I2(aq) + 2Cr3+(aq) + 7H2O(l) (1)

I2(aq) + 2S2O32-(aq)  2I-(aq) + S4O62-(aq) (2)
2I-(aq) + Cu2+(aq)  I2(aq) + CuI(s) (3)
The solubility of iodine in water is poor. Adding an amount of iodide solution to water enhance
the solubility of iodine. Iodine combines with the iodide ion to form highly soluble triiodide ion
and it then reacts with thiosulphate ion as follows:

I2(s) + I-(aq)  I3-(aq)

I3-(aq) + 2S2O32-(aq)  3I-(aq) + S4O62-(aq)
The triiodide ion enters the helical structure of the cellulose polymer and forms a dark blue
complex with the polymer. This interaction, therefore, makes an aqueous solution of starch an
excellent indicator in iodometric and iodimetric determinations.
(a) Preparation of a standard K2Cr2O7 solution (~ 0.02 M)

Procedure: Weigh out accurately about 0.5884 g of K2Cr2O7 and transfer it in a 100 mL
volumetric flask. Dissolve the weighed K2Cr2O7 by shaking well in distilled water and make it up
to the mark of the flask. Calculate the exact concentration of the prepared K2Cr2O7 solution.

(b) Standardization of a given Na2S2O3 solution (~ 0.1 M) with a standard K2Cr2O7 solution (~
0.02 M)
Procedure: Take 50 mL of distilled water in a conical flask, add 10 mL of 10% iodate free KI
solution and 1-2 g of pure solid NaHCO 3. Sake the flask until the NaHCO 3 has dissolved. Add
about 5 mL of conc. HCl acid slowly whilst rotating the flask gently. Make sure that the solution
is acidic. Pipette out 10 mL of the standard K 2Cr2O7 solution and add it into the flask. Cover the
flask with a watch glass and leave it in dark for 5 minutes in order to complete the reaction. At
the end of the period rinse the watch glass and the sides of the flask with distilled water and
titrate the liberated iodine with Na2S2O3 solution. When most of the iodine has reacted (as
indicated by the solution colour which becomes yellowish green), add 8-10 drops of starch
solution and continue the titration drop wise until one drop of Na 2S2O3 solution changes the
colour to light green. Repeat the titrations for two / three more times. Record your burette
reading to two decimal places. Calculate the concentration (in M) of the supplied Na 2S2O3
solution.
Calculation: Suppose in experiment no. 8(b), 9.30 mL supplied Na 2S2O3 solution is required to
titrate the liberated I2 by 10 mL standard K2Cr2O7 solution (0.0200 M). What is the concentration
of the supplied Na2S2O3 solution?

Number of moles solute

Concentration (or strength) of a solution = ---------------------------------- moles/L (= M)

Volume of solution in liter

Now, amount of K2Cr2O7 = concentration × volume in liter

= 0.0200 × 10 × 10-3 mol

= 0.2000 × 10-3 mol

Therefore, amount of Na2S2O3 = 6 × 0.2000 × 10-3 = 1.2000 × 10-3 mol

[ ∵ 1 mol Cr2O72- = 6 mol Na2S2O3, see reaction (1) & (2)]

1.2000 × 10-3 mol

Concentration of supplied Na2S2O3 solution = ----------------------- = 0.1290 M

9.30 × 10-3 L
Experiment No. 4: Determination of the pH-neutralization curves of a strong acid by a
strong base

Principle: When alkali solution is gradually added to an acid solution, the pH of the solution
increases due to removal of H + ions. At the end point there is a sharp increase in the value of pH.
The curve showing the variation of pH with the amount of alkali added is called the pH-
neutralization curve. The end point is marked by point of inflection in the curve. Further,
knowledge of this curve allows selection of appropriate acid-base indicators for titration. The pH
of a solution can also be determined by the emf technique. For this purpose a pH meter will be
used.

Procedure:

1. Take 10 mL of the supplied HCl solution (~ 0.1 M) in a beaker, dilute to about 200 mL.

2. Place the electrode of the pH meter in the above solution.

3. Charge a burette with the supplied 0.2 M NaOH

solution.

4. Add about 0.5 mL aliquot from the burette to

the solution in the beaker. Stir the solution,
and measure its pH.
5. Tabulate burette readings, volume of alkali
(mL) added, and pH of the solution.
6. Plot pH vs. volume of NaOH solution added.
Draw a smooth curve. Locate the end point.
7. Calculate the concentration of supplied HCl
solution.