IISER THIRUVANANTHAPURAM

School of Chemistry
CHY112

Chemistry Laboratory I
Manual_Part 1_Inorganic Chemistry

VARSHA-2024

Name:

Roll No:

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General Instructions

 Come to the lab in time and be prepared for the day's work
 Avoid loose talks and use of mobile phones in the laboratory.
 Always use laboratory coats and goggles. While handling hazardous chemicals use masks
and gloves.
 Do not smell chemicals by placing your nose at the bottle’s opening; waft the smell
toward your nose with your hand. Do not inhale vapors or make skin contact with any
substances.
 Never eat or drink in the lab.
 Waste should be disposed of in the appropriate containers:
 All accidents and dangerous occurrences must be reported immediately and staff in
charge of the laboratory must record all incidents in the accident book. An emergency
shower is located in the foyer area and also there are eyewash stations. The first aid box
is kept in the lab. You should ensure that you know a general fire practice, whom to
contact and where to go in an emergency.
 Students are expected to keep the laboratory and work bench clean. All students should
clean the apparatus and work bench after the work is over. Remove all protective
clothing and wash your hands before leaving the laboratory.
 All pre-lab work must be finished before the relevant laboratory session. Students not
completing the pre-laboratory task will be turned away from the laboratory until the
exercises are completed. Laboratory work in chemistry can be stimulating to students
who appreciate the challenge it offers to their abilities.
 Plan exercise, design procedure and perform experiments to improve the working
efficiency in groups.
 Good time management is the key to success in most areas of IISER life
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CONTENTS

Experiment 1: Titrimetric Estimations Based on Acid-Base Chemistry [1 Session]

(a) Standardization of HCl solution using N/20 oxalic acid solution

(b) Estimation of alkali content in commercial antacid

Experiment 2: Redox-Titrimetric Estimations Based on Permanganometry [2 Session]

(a) Standardization of potassium permanganate using sodium oxalate

(b) Preparation of K3[Fe(C2O4)3]·3H2O

(c) Estimation of the oxalate content of Potassium trisoxalatoferrate(III) trihydrate

Experiment 3: Complexometric Estimations Based on EDTA [1 Session]

(a) Standardization of EDTA solution using a standard zinc acetate solution

(b) Estimation of amount of calcium and magnesium in a milk sample

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 Experiment 1: Acidimetry & Alkalimetry
When the strength of an acid is determined with the help of a standard solution of base, it is
known as acidimetry. Similarly, when the strength of a base (alkali) is determined with the help
of a standard solution of an acid, it is known as alkalimetry. Both these titrations involve
neutralisation of an alkali. In these titrations H+ ions of the acid combine with OH– ions of the
alkali to form unionised molecules of water.

HA + BOH → BA + H2O

or H+ + OH– → H2O

The end point in these titrations is determined by the use of organic dyes (Indicator) which are
either weak acids or weak bases. These change their colours within a limited range of hydrogen
ion concentrations, i.e., pH of the solution. Phenolphthalein is a suitable indicator in the titrations
of strong alkalies (free from carbonate) against strong acids or weak acids, Methyl orange is used
as an indicator in the titrations of strong acids against strong and weak alkalis. No indicator gives
correct results in the titrations of weak acids against weak bases. Such titrations are performed
by some other methods.

Precautions

 Always rinse the burette and the pipette with the solutions to be taken in them.
 Never rinse the conical flask with the experimental solutions.
 Remove the air gaps if any, from the burette
 Never forget to remove the funnel from the burette before noting the initial reading of the
burette.
 Lower end of the pipette should always remain dipped in the liquid while sucking the
liquid.

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Estimation of Alkali Content in Commercial Antacid

Antacid generally contains weakly basic substances such as Al(OH)3, Mg(OH)2, MgCO3 etc.
Alkali content of the antacid is determined by dissolving a weighed quantity of an antacid in
measured excess of standard HCl solution followed by back titration of the excess HCl with a
standard NaOH solution.

Mg(OH)2 + 2HCl = MgCl2+2H2O

Al(OH)3 + 3HCl = AlCl3+3H2O

HCl ≡ ½ Mg(OH)2 ≡ 1/3 Al(OH)3 ≡ 1 equivalent.

∴ 1000mL (N) HCl solution ≡ 58.32/2 = 29.16g of Mg(OH)2≡ 78/3 = 26g of Al(OH)3.

a) Standardisation of sodium hydroxide

Procedure:
Weigh out accurately 0.06 - 0.07g of A.R. crystalline oxalic acid into a 100mL volumetric
flask. Dissolve and dilute up to the mark with distilled water and then mix uniformly. Pipette
out an aliquot of 20mL of the standard oxalic acid in a 250mL conical flask and add one drop
of phenolphthalein indicator. Titrate the solution with the NaOH solution until a light pink
colour appears.

Normality of NaOH solution =

a) Standardization of hydrochloric acid

Pipette out an aliquot of 20mL of the HCl solution in a 250mL conical flask and add one drop of
phenolphthalein indicator. Titrate the solution with the standard NaOH solution until a light pink
colour appears. Repeat the titration until you get concordant values.

Normality of HCl solution =

b) Estimation of alkali content in antacid

Transfer the given antacid suspension to a 100mL volumetric flask using funnel and glass rod.
Make up it into 100 ml with distilled water. Pipette out 20 ml solution into a 250 mL conical
flask. Pipette out 40 mL of the standard 0.2N HCl solution to the conical flask and mix it well.

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Keep it for 15 minutes with occasional shaking. Add one drop of phenolphthalein indicator and
titrate the solution with the standard NaOH solution until a light pink colour appears. Repeat the
titration until you get concordant values.

Calculation

Standardisation of HCl

Sl.No. Vol. of Burette reading Vol. of NaOH

Hydrochloric reacted with HCl
Initial Final
acid(ml) (ml)

1 20

2 20

3 20

Estimation of Antacid (Back titration)

Sl.No. Vol. of HCl (ml) Burette reading Vol. of NaOH

reacted with
Initial Final
unreacted HCl (ml)

1 40

2 40

3 40

Volume of HCl reacted with 20ml antacid solution

1000mL (N) HCl solution ≡ 58.32/2 = 29.16g of Mg(OH)2≡ 78/3 = 26g of Al(OH)3.

Report

Amount of alkali content in the antacid Mg(OH)2 / Al(OH)3 =

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Experiment No. 2: Redox Titrimetric Estimations Based On Permanganometry

These are titrations in which potassium permanganate is used as an oxidizing agent in acidic
medium. The medium is maintained by the use of dilute sulphuric acid. The potential equation,
when potassium permanganate acts as an oxidizing agent, is:

2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O]

or MnO4– + 8H+ + 5e- → Mn2+ + 4H2O (E0 = 1.51V)

From which it follows that equivalent weight is one-fifth of the formula weight, is 31.606 g. The
standard potential in acid solution 𝐸 0 has been calculated to be 1.51 volts, hence permanganate
ion in acid solution is a strong oxidizing agent. . Potassium permanganate acts as a self-indicator.
Before the end point, the solution remains colourless, but after the equivalence point only one
extra drop of KMnO4 solution imparts pink colour, i.e., appearance of pink colour indicates the
end point.

Sulphuric acid is the most suitable acid as it has no action on permanganate ion in dilute
solution. But hydrochloric acid give the reaction.

- - + 2Mn++ + 5Cl2 + 8H2O

2MnO4 + 10 Cl + 16H

Some permanganate may be consumed in the formation of chlorine. With a small excess of free
acid, a very dilute solution, low temperature and slow titration with constant shaking, the
danger from this reaction cause is minimized.

Preparation of Potassium trisoxalatoferrate(III) trihydrate.

Weigh about 1g of Fe(NH4)2(SO4)2·6H2O in a 150-mL conical flask and note down the weight.
Dissolve it in 3mL distilled water and add 1-2 drops of 3M H2SO4. Add 10mL 0.5 M H2C2O4 to
this solution and heat to boiling while stirring constantly to prevent bumping. Remove the
conical flask from the heat and allow the yellow precipitate of FeC2O4 to settle. Decant the
supernatant liquid (pour the liquid away from the solid) and wash the precipitate using 5mL of
hot distilled water. Swirl the mixture and allow the precipitate to settle; decant and repeat the
washing once more.

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Add 4mL of 1M K2C2O4 to the flask containing the precipitate, stir and heat to 40°C. While the
temperature is at 40°C, immediately add 2mL of 6% H2O2 drop wise and stir continuously.
Periodically check the temperature of the solution and make sure that it is at least 40°C (but not
>50°C) during the addition of H2O2. (Some brown Fe(OH)3 may precipitate at this time.)

Heat the resulting solution to boiling. Obtain 4mL of 0.5M H2C2O4 and add 1mL of it all at once
to the boiling solution. Stir continuously and add the last few mL drop wise while maintaining
the temperature near boiling. The solution should turn clear green. If some brown residue
remains, add an additional 1mL of H2C2O4 drop wise, again while the solution is boiling, until the
solution is clear green. However, if the residue that remains is yellow, it is probably unreacted
FeC2O4, and more H2O2 should be added carefully.

If the solution is cloudy, gravity filter it into a clean Erlenmeyer flask. If it is clear, no filtration is
necessary. Then, while swirling constantly, slowly add 3-4mL ethanol to the solution. Allow to
cool, while an ice bath is prepared. Immerse the bottom portion of the flask in the ice bath and
stir slowly until crystals begin to form. Stop stirring and allow the solution to stand in the ice
bath for 20 minutes. A good crop of crystals should have formed before the solution is filtered.

Filter at the pump. Wash with 10ml 1:1 ethanol and dry. Transfer the crystals to a pre-weighed,
labeled dry sample vial and record the weight of the product. This product should store for
further analysis.

Report

Weight of K3 [Fe(C2O4)3]·3H2O =

Percent yield =

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Estimation of the Oxalate Content of K3[Fe(C2O4)3]·3H2O

Standard solution of potassium permanganate is used to analyze the oxalate content of the
potassium trisoxalatoferrate(III)trihydrate, K3[Fe(C2O4)3]·3H2O. In acid solution, potassium
trisoxalatoferrate(III) provides Iron(III) and oxalate ions. Iron(III) is not oxidized by
permanganate ion so the oxalate can be titrated directly. However, oxalate ions react only
slowly with permanganate ions at room temperature so the solution must be warmed to about
60 ºC in order to make the reaction fast enough to be useful in a titration.

2MnO4- + 5C2O42- +16H+ = 2 Mn2++ 10CO2 + 8H2O

Standardisation of potassium permanganate

Weigh out accurately 0.63g A.R. crystalline oxalic acid into a 100mL volumetric flask, dilute up
to the mark with distilled water and then shake to form a uniform solution. Pipette out an
aliquot of 20mL standard oxalic acid solution in a 250mL conical flask. Add 20mL 4N H2SO4, heat
nearly to 70º- 80ºC and then titrate the solution with the 0.1N KMnO4 solution in hot condition
until a faint pink colour stable for 30 seconds is obtained. Record the titre value.

Estimation of the oxalate content

Weigh accurately about 0.04 g of the potassiumtrisoxalatoferrate(III) complex. Boil the sample
with 15 mL of 2 N sulfuric acid in a conical flask. Allow the solution to cool to about 60°C and
titrate slowly with the standard potassium permanganate solution. Continue titration until the
warm solution retains a slight pink colouration for 30sec. Record the titre value. Calculate the
percentage by weight of oxalate in the complex, compare this with the theoretical value and
thus obtain the percentage purity of the complex. (1 ml 1 N KMnO4 = 0.044 g of C2O42- ).

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Calculation

Standardization of KMnO4

Burette reading Vol. of KMnO4

Vol. of oxalic
Sl. No. reacted with H2C2O4
acid(ml) Initial Final (ml)

1 20

2 20

3 20

Estimation of Oxalate Content

Sample 1 Sample 2

Mass of complex taken

Volume of KMnO4 titrated

Volume of 0.1N KMnO4 equivalent to ……. normal KMnO4

Mass of oxalate in the complex

Percentage of oxalate in the complex

Report

Weight of Oxalate in the complex:

Sample I =

Sample II =
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 EXPERIMENT 3: COMPLEXOMETRIC ESTIMATIONS BASED ON EDTA

A titration, in which an undissociated complex is formed at the equivalence point, is called

complexometric titrations. These titrations are superior to precipitation titrations as there is no
error due to co-precipitations. EDTA (ethylenediamine tetra-acetic acid) is a useful reagent
which forms complexes with metals. In the form of disodium salt, it is used to estimate various
metal ions in presence of eriochrome black-T or other suitable metal ion indicator.

To simplify the discussion, ethylenediaminetetra-acetic acid is assigned by the formula H4Y: and
the sodium salt is Na2H2Y and affords the complex forming ion H2Y2- in the aqueous solution.
The usefulness of EDTA as the titrant is due the presence of six atoms which are available for
co-ordination to the metal ions in such a way that five membered rings are formed. 1:1
complexes are usually formed and these are the most important and the reactions with M ++
cations may be written as

The ionization of the complex is dependent upon the 𝑝𝐻 of the solution. Lowering of the pH
decreases the stability of the metal-EDTA complex. The more stable the metal-EDTA complex,
the lower is the 𝑝𝐻 at which an EDTA titration is possible.

Let us consider the metal ion indicator which forms 1:1 complexes. The use of metal ion
indicator in an EDTA titration may be written as

M – In + EDTA ⟶ M – EDTA + In

This reaction will proceed if the metal indicator complex is less stable than metal-EDTA complex.
During titration the metal ions are progressively complexed by EDTA until ultimately the metal
is displaced from the complex M – In to leave the free indicator (In).

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Thus Eriochrome Black T, which may be written as H2In- exhibits the following acid base
behavior.

pH -- pH ---
- HIn In
H2In
5.3- 7.3 10.5 - 12.5
Red Blue Yellow-orange

4. 2. Estimation of Calcium in Milk

4. 2. 1. Standardization of EDTA

Prepare 0.01M zinc sulphate solution in 100ml volumetric flask. Pipette out 20mL of standard
zinc sulphate solution in a 250mL conical flask, dilute it to 100mL with deionized water, add 2mL
of NH3-NH4Cl buffer solution and a pinch of eriochrome black T indicator when the colour of the
solution turns wine red. Titrate the solution with the EDTA solution until wine red colour turns
pure blue.

The last trace of a reddish shade should disappear at the end point. Titrate slowly near the end
point.

4. 2.2 Estimation of Calcium in Milk

Pipette out 20mL of the supplied milk solution in a 100mL beaker, precipitate proteins of milk
by trichloroacetic acid and filter into 100mL volumetric flask. Wash with deionised water, dilute
up to the mark with deionised water and mix uniformly. Pipette out 20mL of the diluted supplied
milk solution in a 250mL conical flask, dilute to 100mL with deionised water, add 2mL of NH3-
NH4Cl buffer solution and a pinch of Eriochrome Black-T indicator when the colour of the
solution turns wine red. Titrate the solution against the EDTA solution until the wine red colour
turns pure blue. No tinge of reddish blue should remain at the equivalence point. Titrate slowly
near the end point. (1mL (M) EDTA = 0.04008g of Ca).

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Standardization of EDTA

Sl.No. Vol. of ZnSO4 Burette reading Vol. of EDTA

(ml) Initial Final (ml)

1 20

2 20

3 20

Estimation of Ca2+

Sl.No. Vol. of Ca2+ Burette reading Vol. of EDTA

(ml) Initial Final (ml)

1 20

2 20

3 20

Report

Percentage of calcium in the supplied milk is ………….

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