Experiment #: 01

Experiment Title: Preparation of 0.1M sodium carbonate, Na2CO3 solution and standardization of
hydrochloric acid, HCl solution against sodium carbonate (Na2CO3) solution. (Strong acid vs. Weak
base)
Objectives:

1. To demonstrate the basic laboratory technique of titration

2. To learn to calculate molarity of an unknown acid or base, by neutralizing it with a measured quantity of a
base or acid solution whose concentration is known.

Theory:

The experiment is based on acid-base titration to determine the end point at which the reaction is completed
i.e. the volume of acid which is required to neutralize the base solution.
In this experiment the following reactions are occurred:
Na2CO3(aq) + HCl = NaHCO3(aq) + NaCl(aq)
NaHCO3(aq) + HCl= NaCl +H2O + CO2
So the ultimate reaction is,
Na2CO3(aq) + 2 HCl = 2 NaCl(aq) +H2O + CO2

List of Equipment:

Apparatus Chemicals

1. Volumetric flask (100ml) 1. Na2CO3

2. Burette 2. HCl solution
3. Pipette (10ml) & Pipette Filler 3. Methyl Orange Indicator
4. Conical flask (250ml) 4. Distill Water
5. Stand & Clamp
6. Balance
7. Wash Bottle
8. Dropper
9. Funnel
Procedure:

● Prepare 0.1M standard solution of Na2CO3 by weighing required amount of solid Na2CO3 in the volumetric
flask.
●Take 10ml of standard Na2CO3 solution in a conical flask by pipette and add approximately 50ml water.
●Add 3-4 drops of methyl orange indicator so the solution becomes yellow in color.
●Take the initial burette reading and start the addition of HCl from the burette. Note the burette reading when
just one drop of HCl changes the color of the solution from yellow to faint pink (orange color). Note the
burette reading.
●The difference of the burette reading from initial to the final reading will be the volume of acid required in
the titration.
● Repeat the experiment till three concordant value of HCl used is obtained.
●Calculate the strength of HCl and then find out the molarity of commercial HCl acid.

Page 39 of 40
Data Collection:

Table: Standardization of HCl against standard Na2CO3 solution.

No of Volume of Burette reading Difference Average
observations Na2CO3 volume of
(ml)
HCl
(ml)
(ml)
IBR FBR
1

Calculation:
Molecular Weight of Na2CO3 = 23x2+12+16x3
= 106
1000 ml 1M Na2CO3 solution contains = 106g.
106x100x0.1
100 ml 0.1M Na2CO3 solution contains = ----------------------------------
1000
= 1.06g.
Now we know,
Amount of acid= Amount of alkali Here,
𝑀𝑎 𝑉𝑎 ÷ 𝑛𝑎 = 𝑀𝑏𝑉𝑏 ÷ 𝑛𝑏 Molarity of acid HCl ,Ma =
Volume of acid HCl ,Va =
Molarity of alkali Na2CO3, Mb =
Volume of alkali Na2CO3 ,Vb =
No. of moles of acid, na=
No. of moles of alkali, nb=
Result:
The strength / molarity of HCl =…………M
Report:
The report will contain all the data you have recorded in your rough copy along with the theory. No need to
write the experimental procedure.

Text Book:
1. General Chemistry
Darrell Ebbing , Steven D. Gammon
9th Edition Cengage Learning, 2007.

Reference Book:
1. Vogel’s Textbook of Quantitative Chemical Analysis
Page 39 of 40
 G.H. Jeffery , J.Bassett, J. Mendham, R.C. Denney.
5th edition.

Experiment #: 02
Experiment Title: Preparation of 0.1M sodium hydroxide, NaOH solution and standardization of
hydrochloric acid, HCl with standard NaOH solution. (Strong acid vs. Strong base)

Objectives:

1. To demonstrate the basic laboratory technique of titration

2. To learn to calculate molarity of an unknown acid or base, by neutralizing it with a measured quantity of a
base or acid solution whose concentration is known.

Theory:

The experiment is based on acid-base titration to determine the end point at which the reaction is completed
i.e. the volume of acid which is required to neutralize the base solution.
In this experiment the following reaction is occurred:
NaOH(aq) + HCl(aq) = NaCl (aq) + H2O

List of Equipment:

Apparatus Chemicals

1. Volumetric flask (100ml) 1. NaOH pelletes

2. Burette 2. HCl solution
3. Pipette (10ml) & Pipette Filler 3. Methyl Orange Indicator
4. Conical flask (250ml) 4. Distill Water
5. Stand & Clamp
6. Balance
7. Wash Bottle
8. Dropper Page 39 of 40
 9. Funnel

Procedure:

● Prepare 0.1M standard solution of NaOH weighing required amount of solid NaOH in the volumetric flask.
●Take a 10ml of standard NaOH solution in a conical flask by pipette and add approximately 50ml of water.
●Add 3-4 drops of methyl orange indicator so the solution becomes yellow in color.
●Take the initial burette reading and start the addition of HCl from the burette. Note the burette reading when
just one drop of HCl changes the colour of the solution from yellow to faint pink (orange color). Note the
burette reading.
●The difference of the burette reading from initial to second end point will be the volume of acid required in
the titration.
● Repeat the experiment till three concordant value of HCl used is obtained.
●Calculate the strength of dil. HCl and then find out the molarity of commercial HCl acid.

Data Collection:
Table: Standardization of HCl against standard NaOH solution.

No of Vol. of NaOH Burette reading Difference Average

obs (ml) (ml) volume of
(ml)
HCl (ml)
IBR FBR

Calculation:

Molecular weight of NaOH = 23+16+1

= 40
1000 ml 1M NaOH solution contains = 40g.

40x100x0.1
100 ml 0.1M NaOH solution contains = -----------------------
1000
Page 39 of 40
 = 0.4g
Now we know,
Amount of acid= Amount of alkali Here,
𝑀𝑎 𝑉𝑎 ÷ 𝑛𝑎 = 𝑀𝑏𝑉𝑏 ÷ 𝑛𝑏 Molarity of acid HCl ,Ma =
Volume of acid HCl ,Va =
Molarity of alkali NaOH, Mb =
Volume of alkali NaOH ,Vb =
No. of moles of acid, na=
No. of moles of alkali, nb=
Result:
The strength / molarity of HCl =…………M

Report:
The report will contain all the data you have recorded in your rough copy along with the theory. No need to
write the experimental procedure.

Page 39 of 40
Experiment #: 03
Experiment Title: Preparation of 0.05M oxalic acid, C2H2O4 solution and standardization of sodium
hydroxide, NaOH solution against oxalic acid. (Strong base vs. Weak acid)

Objectives:

1. To demonstrate the basic laboratory technique of titration

2. To learn to calculate molarity of an unknown acid or base, by neutralizing it with a measured quantity of a
base or acid solution whose concentration is known.

Theory:

The experiment is based on acid-base titration to determine the end point at which the reaction is completed
the volume of acid which is required to neutralize the base solution.
In this experiment the following reactions are occurred:
COO-Na
HOOC-COOH + 2 NaOH = +2 H2O
COO-Na

List of Equipment:
Apparatus Chemicals

1. Volumetric flask (100ml) 1. NaOH pelletes

2. Burette 2. C2H2O4
3. Pipette (10ml) & Pipette Filler 3. Phenolphthalein Indicator
4. Conical flask (250ml) 4. Distill Water
5. Stand & Clamp
6. Balance
7. Wash Bottle
8. Dropper
9. Funnel

Procedure:

● Prepare 0.05M standard solution of C2H2O4 by weighing required amount of C2H2O4 in volumetric flask.
●Take 10ml of standard C2H2O4 solution in a conical flask by pipette and add 50ml water approximately.
●Add 3-4 drops of phenolphthalein indicator and the solution will not change the color.
●Take the initial burette reading and start the addition of NaOH from the burette. Note the burette reading
when just one drop of NaOH changes the color of the solution from no color to purple. Note the burette
reading.
●The difference of the burette reading from initial to end point will be the volume of alkali required in the
titration.
● Repeat the experiment till three concordant value of NaOH used is obtained.
●Calculate the strength of dill NaOH and then find out the molarity of commercial NaOH acid.

Data Collection: Page 39 of 40

Table: Standardization of NaOH against standard C2H2O4 solution.

No of Vol. of Burette reading (ml) Difference Average

observations C2H2O4 (ml) (ml) volume of
NaOH (ml)
IBR FBR

Calculation:
Molecular Weight of C2H2O4 . 2H2O = 12×2+1×2+16×4+36
= 126
1000 ml 1M C2H2O4 solution contains = 126g.
126x100x0.05
100 ml 0.05M C2H2O4 solution contains = ----------------------------------
1000
= 0.63g.
Now we know,
Amount of acid= Amount of alkali Here,
𝑀𝑎 𝑉𝑎 ÷ 𝑛𝑎 = 𝑀𝑏𝑉𝑏 ÷ 𝑛𝑏 Molarity of acid C2H2O4,Ma =
Volume of acid C2H2O4 ,Va =
Molarity of alkali NaOH, Mb =
Volume of alkali NaOH ,Vb =
No. of moles of acid, na=
No. of moles of alkali, nb=

Result:

The strength / molarity of NaOH =………M

Report:
The report will contain all the data you have recorded in your rough copy along with the theory. No need to
write the experimental procedure.

Page 39 of 40
Page 39 of 40
Experiment #: 04
Experiment Title: Preparation of 0.02M potassium dichromate, K2Cr2O7 solution and standardization
of sodium thiosulphate, Na2S2O3 solution against standard potassium dichromate solution.
Objectives:

1. To demonstrate the basic laboratory technique of iodometric titration

2. To learn to calculate molarity of an unknown substance, by using redox reaction.

Theory:
The oxidation and reduction process in this experiment involve iodine and therefore the process is known as
iodometric titration. Here the strength of Na2S2O3 solution is to determine with the help of standard K2Cr2O7
solution.
In this experiment K2Cr2O7 is reduced by an acidic solution of potassium iodide and iodine is liberated as
below:
Cr2O7 2-
+ 6I- + 14H+ = 2Cr3+ + 3I2 +7H2O
The liberated Iodine reacts with thiosulphate solution rapidly as
2S2O3 2- + I2 = S4O6 2- +2I-
2S2O3 2- + I3 = S4O6 2- +3I-
Now, from the above reactions we can write,
6S2O32- = Cr2O7 2-
List of Equipment:
Apparatus Chemicals

1. Volumetric flask (100ml) 1. Na2S2O3

2. Burette 2. K2Cr2O7
3. Pipette (10ml) & Pipette Filler 3. NaHCO3
4. Conical flask (250ml) 4. KI
5. Stand & Clamp 5. HCl
6. Balance 6. Starch solution
7. Wash Bottle 7. Distilled Water
8. Dropper
9. Funnel
Procedure:

● Prepare 0.02M standard solution of K2Cr2O7 by weighing required amount of K2Cr2O7 in volumetric flask.
●Take about 50ml distilled water in a conical flask.
●Add 10ml 10% Iodate free (KI) Potassium Iodide and 1-2gm pure sodium Hydrogen Carbonate and shake
flask until the salt dissolve.
●Add about 5ml conc. HCl slowly and add 10ml standard K2Cr2O7 solution by means of a pipette in the flask.
●Shake the flask and cover it with a watch glass; allow the solution to stand for about five minutes in the dark
(inside the desk).
●Titrate the liberated Iodine with sodium thiosulphate solution from a burette until the brown color fades
(light yellow).
●Add about 6-7 drops of starch solution and continue titration by adding sodium thiosulphate solution from
the burette until one drop of sodium thiosulphate solution changes the color of the solution from deep blue to
light green or light blue. This is the end point.
Page 39 of 40
● Repeat the experiment till three concordant value of Na2S2O3 used is obtained.
●Calculate the strength of sodium-thiosulphate and then find out the molarity of commercial sodium-
thiosulphate.
Data Collection:
Table: Standardization of sodium-thiosulphate against standard potassium dichromate solution.

No of Vol. K2Cr2O7 Burette reading Difference Average

obs of (ml) (ml) volume of
(ml)
Na2S2O3
IBR FBR (ml)

Calculation:
Molecular weight of K2Cr2O7 = 39x2+52x2+16x7
= 294gm
1000 ml 1M K2Cr2O7 solution contains = 294g.

294x100x0.02
100 ml 0.02M K2Cr2O7 solution contains = -------------------
1000
= 0.588g
Now we know,
Amount of K2Cr2O7= Amount of Na2S2O3
𝑀𝑎 𝑉𝑎 ÷ 𝑛𝑎 = 𝑀𝑏𝑉𝑏 ÷ 𝑛𝑏 Here,
Molarity of K2Cr2O7,Ma =
Volume of K2Cr2O7 ,Va =
Molarity of Na2S2O3, Mb =
Volume of K2Cr2O7 ,Vb =
No. of moles of K2Cr2O7, na=
No. of moles of K2Cr2O7, nb=

Result:
The strength of Na2S2O3 =…………….M

Report:
Page 39 of 40
The report will contain all the data you have recorded in your rough copy along with the theory. No need to
write the experimental procedure.

Page 39 of 40
Experiment #: 05
Experiment Title: Determination of Iron, Fe (II) in a supplied sample solution using standard solution
of potassium permanganate, KMnO4.
Objectives:
1. To demonstrate the basic laboratory technique of redox titration.
2. To learn to calculate molarity of an unknown substance, by using redox reaction.
Theory:
This experiment involves the oxidation and reduction of iron and potassium permanganate and hence known
as oxidation-reduction titration. In presence of sulphuric acid, potassium permanganate acts as an oxidizing
agent. On the other hand, ferrous ion (Fe2+) is a reducing agent. Therefore, when potassium permanganate is
added to it, ferrous ion (Fe2+) is oxidized to ferric ion and potassium permanganate is reduced to manganous
ion, Mn2+.

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

10FeSO4 + 5H2SO4 + 5[O] = 5Fe2(SO4)3 + 5H2O

2KMnO4 +10 FeSO4+8 H2SO4 = K2SO4+2MnSO4 +5Fe2(SO4)3 + 8H2O

Ionic from of the above equation,

MnO4- +8H+ +5e = Mn2+ +4H2O
5Fe2+ = 5 Fe3+ +5e
MnO4- + 8H+ +Fe2+ = Mn2+ +5Fe3+ +4H2O
Or MnO4- = 5Fe3+ = 5e

List of Equipment:
Apparatus Chemicals

1. Volumetric flask (100ml) 1. Green Vitriol [FeSO4.7H2O]

2. Burette 2. 1M H2SO4
3. Pipette (10ml) & Pipette Filler 3. Standard KMnO4 Solution
4. Conical flask (250ml)
5. Stand & Clamp
6. Balance
7. Wash Bottle
8. Dropper
9. Funnel

Procedure:

● Prepare 0.1M ferrous salt solution by weighing required amount of green vitriol in volumetric flask. To
prepare this solution use 80ml 1M H2SO4 and rest of the amount of distill water.
● Take a 10ml of ferrous salt solution in a conical flask by pipette. No need to add any indicator as KMnO 4
acts as self indicator.
●Take the initial burette reading and start the addition of standard KMnO4 solution from the burette. Note the
burette reading when just one drop of KMnO4 changes the color of the solution from no color to faint pink.
Note the burette reading.
●The difference of the burette reading from initial to second end point will be the volume of acid required in
the titration.
● Repeat the experiment till three concordant value of KMnO4 used is obtained.
●Calculate the amount of iron in the prepared iron solution.
Page 39 of 40
Data Collection:
Table: Determination of the amount of Fe2+ ion using standard KMnO4

Burette reading of KMnO4 (ml)

No. of Vol. of Difference Average
observations supplied IBR FBR of KMnO4
Ferrous KMnO4used used (ml)
solution (ml) (ml)
1

Calculation:
Molecular weight of FeSO4.7H2O = 278 g
1000ml 1M FeSO4 solution contains =278g

100ml 0.1M ,, ,, = 278x100x0.1

1000
= 2.78 g

Suppose, volume of required KMnO4 solution = **ml

Theoretically, 1000ml of 1M KMnO4 solution = 5 x 55.84 Fe2+
1ml of 1M KMnO4 solution = 5 x 0.05584 g Fe2+
**ml 0.02M KMnO4 solution = 5 x 0.05584 x ** x 0.02 g Fe2+
= ***g Fe2+

Therefore, 10ml of dilute ferrous salt solution contains *** g of Fe2+

100ml ,, ,, ,, ,, ,, ***x 100 g Fe2+
10
= ****g of Fe2+

Result:
The supplied ferrous salt solution contains ****g of Fe2+

Report:
The report will contain all the data you have recorded in your rough copy along with the theory. No need to
write the experimental procedure.

Page 39 of 40
Page 39 of 40
Experiment #: 06
Experiment Title: Estimation of Copper, Cu2+ contained in a supplied solution with standard sodium
thiosulphate, Na2S2O3 solution.
Objectives:

1. To demonstrate the basic laboratory technique of iodometric titration

2. To learn to calculate the amount of copper in the supplied solution.

Theory:
This experiment comes under the category of iodometry which is used widely in the analysis of ores, alloys
etc.
When an excess of KI is added to the solution containing Cu2+ in neutral or slightly acidic medium, quantitative
liberation of iodine takes place.

2CuSO4.5H2O + 4KI→ 2CuI2 + 2K2SO4 + 5H2O

2CuI2 →Cu2I2 + I2

This liberated iodine is then titrated against standard Na2S2O3 solution using starch solution as indicator near
the end point.
2Na2S2O3 + I2 →Na2S4O6 + 2NaI

Ionic equation will be:

2Cu2+ + 2I− → Cu22+ + I2 + 2e
I2 + 2S2O32− + 2e S4O62− + 2I−

From the above equation it is evident that

2Cu2+ ≡ I2 ≡ 2S2O32− ≡ 2e

The equivalent weight of Cu2+ will be one half of twice the molecular weight since the reaction involves two
electrons per two moles of Cu2+.
Eq. wt. of Cu2+ = (2 x 63.5) / 2 = 63.5
The titration fails when any mineral acid is present in the solution and therefore before commencing the
titration the acid should be neutralized. This is done by drop wise addition of NH4OH until a slight blue
precipitate just appears.
H+ + OH−→ H2O
2NH4OH + Cu2+ → 2NH4+ + Cu (OH) 2↓
blue precipitate
The precipitate can be removed by addition of CH3COOH in the solution.
Cu (OH) 2 + 2CH3COOH → Cu2+ + 2CH3COO− + 2H2O

Moreover, the precipitate of Cu2I2 absorbs I2 from the solution and releases it slowly making the detection of
sharp end point difficult. So, a small amount of NH4SCN is added near the end point to displace the absorbed
iodine from Cu2I2 precipitate.

List of Equipment:
Apparatus Chemicals

Page 39 of 40
 1. Volumetric flask (100ml) 1. Na2S2O3
2. Burette 2. K2Cr2O7
3. Pipette (10ml) 3. CuSO4.5H2O
4. Conical flask (250ml) 4. NaHCO3
5. Stand & Clamp 5. KI
6. Balance 6. CH3COOH
7. Wash Bottle 7. NH4SCN
8. Dropper 8. NH4OH
9. Funnel 9. HCl
10. Pipette Filler 10. Starch

Procedure:

Part 1: Standardization of sodium thiosulphate (Na2S2O3) solution with standard K2Cr2O7 solution

● Prepare 0.1M standard solution of K2Cr2O7 by weighing required amount of K2Cr2O7 in volumetric flask.
●Take about 50ml distilled water in a conical flask.
●Add 10ml 10% Iodate free (KI) Potassium Iodide and 1-2gm pure sodium Hydrogen Carbonate and shake
flask until the salt dissolve.
●Add about 5ml conc. HCl slowly and add 10ml standard K2Cr2O7 solution by means of a pipette in the flask.
●Shake the flask and cover it with a watch glass; allow the solution to stand for about five minutes in the dark
(inside the desk).
●Titrate the liberated Iodine with sodium thiosulphate solution from a burette until the brown color fades
(light yellow).
●Add about 6-7 drops of starch solution and continue titration by adding sodium thiosulphate solution from
the burette until one drop of sodium thiosulphate solution changes the color of the solution from deep blue to
light green or light blue. This is the end point.
● Repeat the experiment till three concordant value of Na2S2O3 used is obtained.
●Calculate the strength of sodium-thiosulphate .

Part 2: Estimation of copper

● Pipette out 20 mL of solution in a 250 mL conical flask and neutralized the solution by dropwise addition
of ammonium hydroxide (NH4OH) solution (1:1) until a blue precipitate appears.
● Dissolve the precipitate in acetic acid (CH3COOH) adding about 0.5 mL in excess. Dilute the solution to
about 80 mL and add 20 mL of potassium iodide solution (10%).
● Keep the flask covered with watch glass in a dark and cool place for about 3–5 minutes and titrate the
liberated iodine with standard sodium thiosulphate solution form burette.
● When the colour of the solution fades to a light yellow, add few drops of starch followed by 20 mL of
ammonium thiocyanate (NH4SCN) solution (10%).
● Titrate the solution till the blue colour discharges and a white or flesh white residue is left in the flask.
● Repeat the experiment till three concordant value of Na2S2O3 used is obtained.

Data Collection:
Table 1: Standardization of sodium-thiosulphate against standard potassium dichromate solution (0.1M).
Page 39 of 40
 No of Vol. K2Cr2O7 Burette reading Difference Average
obs of (ml) (ml) volume of
(ml)
Na2S2O3
IBR FBR (ml)

Table 2: Estimation of copper using standard Na2S2O3 solution

No of Volume.of Burette reading (ml) Volume.of Average

observations copper Na2S2O3 volume
solution (ml) solution (ml) (ml)
IBR FBR

Calculation:
A) Standardization of Na2S2O3 solution with standard K2Cr2O7 solution

Molecular weight of K2Cr2O7 = 39x2+52x2+16x7

= 294gm
1000 ml 1M K2Cr2O7 solution contains = 294g.

294x100x0.02
100 ml 0.02M K2Cr2O7 solution contains = -------------------
1000
= 0.588g
Now we know,

Here,
Molarity of K2Cr2O7,Ma =
Page 39 of 40
Amount of K2Cr2O7= Amount of Na2S2O3 Volume of K2Cr2O7 ,Va =
𝑀𝑎 𝑉𝑎 ÷ 𝑛𝑎 = 𝑀𝑏𝑉𝑏 ÷ 𝑛𝑏 Molarity of Na2S2O3, Mb =
Volume of K2Cr2O7 ,Vb =
No. of moles of K2Cr2O7, na=
No. of moles of K2Cr2O7, nb=

B) Estimation of copper
1000 mL of 1(N) Na2S2O3 solution = 63.5 g of copper
1 mL of 1(N) Na2S2O3 solution = 0.0635 g of copper
Y mL of Z(N) Na2S2O3 solution = (0.0635 x Y x Z) g of copper
Y = Volume of Na2S2O3 solution required for the titration of the given copper solution (Ref. - Table 2)
Z = Strength of Na2S2O3 solution
20 mL solution contains (0.0635 x Y x Z) g of copper
1000 mL solution contains [(0.0635 x Y x Z x 1000) / 20] g of copper
= P g (say) of copper

Result:
The amount of copper in the given solution is P g/L.

Report:
The report will contain all the data you have recorded in your rough copy along with the theory. No need to
write the experimental procedure.

Text Book:
1. General Chemistry
Darrell Ebbing , Steven D. Gammon
9th Edition Cengage Learning, 2007.

Reference Book:
1. Vogel’s Textbook of Quantitative Chemical Analysis
G.H. Jeffery, J.Bassett, J. Mendham, R.C. Denney.
5th edition.

Page 39 of 40
Experiment #: 07
Experiment Title: Determination of total hardness of water.

Objectives:
1. To determine the concentrations of Ca2+(aq) and Mg2+(aq) ions in a commercial sample of bottled mineral
water.
2. To compare experimental results with the concentrations of the metal ions claimed by the manufacturer.

Theory:
Natural water always contains a variety of dissolved ions, including Na+, K+, Ca2+, Mg2+, Cl-, HCO3-, and
some other. If concentrations of Ca and Mg ions are relatively large, the water is called hard. The ions
involved in water hardness, i.e. Ca2+(aq) and Mg2+(aq), can be determined by titration with a chelating agent,
ethylenediaminetetraacetic acid (EDTA), usually in the form of disodiumsalt (H2Y2-). The titration reaction
is:

Ca2+(aq) + H2Y2- (aq) ⎯⎯→ CaY2- (aq) + 2H+(aq)

Eriochrome Black T is commonly used as indicator for the above titration. At pH 10, Ca2+(aq) ion first
complexes with the indicator as CaIn+(aq) which is wine red. As the stronger ligand EDTA is added, the
CaIn+(aq) complex is replaced by the CaY2-(aq) complex which is blue. The end point of titration is indicated
by a sharp color change from wine red to blue. Titration using Eriochrome Black T as indicator determines
total hardness due to Ca2+(aq) and Mg2+(aq) ions. Hardness due to Ca2+(aq) ion is determined by a separate
titration at a higher pH, by adding NaOH solution to precipitate Mg(OH)2(s), using hydroxynaphthol blue as
indicator.

List of Equipment:
Apparatus Chemicals

1. Volumetric flask (100ml) 1. Bottled mineral water

2. Burette 2. 0.01 M EDTA
3. Pipette (10ml) 3. Eriochrome Black T indicator
4. Conical flask (250ml) 4. Hydroxynaphthol blue indicator
5. Stand & Clamp 5. Distilled water
6. Balance 6. 50% w/v NaOH solution (50 g in 100 cm3
solution)
7. Wash Bottle 7. pH 10 (NH3-NH4Cl buffer)
8. Dropper
9. Funnel
10. Pipette Filler

Procedure:

Part A: Determination of total hardness

● Pipette 50 cm3 mineral water into a conical flask.
● Add 2 cm3 buffer solution followed by 3 drops of Eriochrome Black T indicator solution.

Page 39 of 40
● Titrate with 0.01 M EDTA until the solution turns from wine red to sky blue with no hint of red (save the
solution for colour comparison).
● Repeat the titration to obtain three concordant results.

Part B: Determination of concentration of Ca2+(aq) ions

● Pipette 50 cm3 of mineral water into a conical flask.
● Add 30 drops of 50% w/v NaOH solution, swirl the solution and wait for a couple of minutes to completely
precipitate the magnesium ions as Mg(OH)2(s).
● Add a pinch of hydroxynaphthol blue (exact amount to be decided by the intensity of the resulting coloured
solution) and titrate with 0.01 M EDTA until it changes to sky blue (save the solution for colour comparison).
● Repeat the titration to obtain two concordant results.

Data Collection:
Table 1: Determination of total hardness
No of Vol. of Burette reading Difference Average
obs mineral water (ml) (ml) volume of
(ml) EDTA(ml)
IBR FBR

Table 2: Determination of concentration of Ca2+(aq) ions

No of Volume of Burette reading (ml) Difference Average

observations mineral water (ml) volume of
(ml) EDTA
IBR FBR (ml)

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Calculation:
1. From the results in Part A, determine the total concentration of Ca2+(aq) and Mg2+(aq) ions in the mineral
water sample in mol dm-3.
2. From the results in Part B, determine the concentration of Ca2+(aq) ions in the mineral water sample in mg
dm-3, or ppm.
3. Hence, calculate the concentration of Mg2+(aq) ions in the mineral water sample in mg dm-3 or ppm.
Compare with the corresponding values displayed on the label of the bottle.

Result:
The concentration of Ca2+(aq) and Mg2+(aq) ions in the mineral water sample is ……mg dm-3and ……mg
dm-3respectively.

Report:
The report will contain all the data you have recorded in your rough copy along with the theory. No need to
write the experimental procedure.

Text Book:
1. General Chemistry
Darrell Ebbing , Steven D. Gammon
9th Edition Cengage Learning, 2007.

Reference Book:
1. Vogel’s Textbook of Quantitative Chemical Analysis
G.H. Jeffery, J.Bassett, J. Mendham, R.C. Denney.
5th edition
8. Determination of Calcium in a Sample of Calcium Carbonate
Objective:—
The main objective of this experiment is to determine the amount of Calcium in a sample of
Calcium Carbonate. As, this experiment involves a redox reaction, it is very helpful to study about
oxidation and reduction theory. This experiment is in fact more important from practical point of
view. Because with the help of this experiment, the amount of calcium (in gram) present in any
substance can be determined. Even percentage of purity of calcium can also be determined.

Theory:—
The amount of calcium in a supplied sample of calcium carbonate is determined in this
experiment. The reaction that occurs here is oxidation and reduction reaction.
An oxidation-reduction reaction (redox) is a reaction in which electrons are transferred between
species or in which atoms change oxidation numbers. Oxidation is the half reaction in which
there is loss of electrons by a species. Reduction is the half reaction in which there is a gain of
electrons by a species (either an atom or an ion).
The reactions involved in this experiment are:
CaCO3 + 2HCl → CaCl2 + H2O + CO2

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 CaCl2 + (NH4)2C2O4 → CaC2O4 +2NH4Cl

CaC2O4 +H2SO4 → H2C2O4 + CaSO4

5H2C2O4 + 2KMnO4 +3H2SO4 →K2SO4 + 2MnSO4 + 10CO2 + 8H2O

In this experiment, KMnO4 is standardized with the help of standard sodium oxalate solution.
The strength of KMnO4 is determined by the following

equation: Vacid × Sacid = Vbase × Sbase

Where, Vacid = volume of acid

Sacid = strength of acid

Vbase = volume of base

Sbase = strength of base

Calcium carbonate is dissolved in acid and then it is precipitated as calcium oxalate. In order to
determine the weight of Calcium, the following equation is used:

1 equivalent weight of KMnO4  1 equivalent weight of Oxalic Acid

 1 equivalent weight of CaC2O4

 1 equivalent weight

of Ca2+ 1000 ml (N) KMnO4 solution  1000 ml (N) calcium

 1 equivalent weight of calcium

 20 gm of Ca+2

So, 1000 ml (N) KMnO4 solution should be equivalent to one-gram equivalent weight that is
20 grams of calcium. Therefore,

1 ml of (N) KMnO4  0.02 gram of calcium

So, the weight of calcium in the supplied calcium carbonate may then be easily calculated
using the above relation.

Apparatus:—

1. Conical flask

2. Burette

3. Pipette

4. Volumetric flask

5. Stand

6. Funnel
Page 39 of 40
 Name of the chemicals used:—

1. Calcium Carbonate (CaCO3)

2. Ammonium Oxalate ((NH4)2C2O4)

3. Sodium Oxalate (Na2C2O4)

4. H2SO4 solution

5. HCl solution

6. KMnO4 solution

7. NH3 solution (1:1)

8. Distilled water

Procedure

Take about 0.1 g calcium salt in a 250 mL beaker. Add about 10 mL distilled water and 4-10 mL of 6
N HCl acid slowly by means of a measuring cylinder to prepare a clear solution. Warm the solution to
drive off CO2. Wash the watch glass and walls of the beaker with distilled water and dilute to about 15
mL. Heat to 60-80 0C and add 6% 50 mL of warm solution of ammonium oxalate. If ammonium oxalate
solution is not clear, filter before using it. Add 3-4 drops of methyl orange indicator. Then introduce
ammonium solution (1:1) dropwise till the color changes from red to yellow. Allow the solution to
stand for about 10-15 minutes to settle the precipitate. Filter the solution through an ordinary filter
paper, wash the beaker and precipitate with distilled water and check chloride with help of silver nitrate.
When it comes free from chloride then dissolved the precipitate in 50 mL of 6 N H2SO4 in a beaker.
Heat it to 80-90 0C if necessary. Transfer to cool solution to a 250 mL volumetric flask and make the
volume up to the mark by adding distilled water. Standardize supplied KMnO4 solution with standard
0.01 N sodium oxalate solution as in Expt. No.9. Take 20 mL of calcium solution and titrate it with
standard KMnO4 solution. Heat the solution up to 60-80 0C. Take the first pink colors that persist for
1-20 second as an end point.

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Data:—

TABLE: 1
(Standardization of Potassium Permanganate solution with Standard Sodium
Oxalate solution)

Number of Volume of Burette reading Volume of Average Strength

KMnO4
Obser- Na2C2O4 Volume of Of
Initial Final
ml KMnO4
-vation ml KMnO4
Reading Reading
ml
ml N
ml

TABLE: 2
(Determination of Calcium Ion by Standard Potassium Permanganate Solution)

Number of Volume Of Burette reading Volume of Average

KMnO4
Obser- Fe2+ Volume of KMnO4 Ml
Initial Final
ml
-vation Solution
Reading Reading
ml
ml ml

Calculation:—
from Vred × Sred = Vox × Sox Here,

VKMnO4 = ml

SNa2C2O4 = N VNa2C2O4 = ml SK2Cr2O7 = N

Again
,
1000 ml (1.0N) KMnO4 = 20 gm Ca+2(20 ml)

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 => ml N KMnO4 = gm Ca+2 (20 ml)

Thus the amount of iron present in 250 ml= (( × 250) / 20) gm

= gm

100 gm CaCO3 contains 40 gm Ca+2

So gm CaCO3 contains gm Ca+2

Result:—

The amount of calcium (in gm) present in the supplied calcium carbonate solution (per
250 ml) is:

WCa = gm.

Percentage of error:

(Known Value – Observed Value) X 100

Percentage of error =

Known value

Known amount of calcium =

gm

Observed amount of iron = gm

Percentage of error = (( – )/ )× 100 %

= %

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Discussion:—

The following causes may be mentioned as the causes for errors:

1) As the calcium solution was not given enough time to precipitate, all the
Calcium might not have been precipitated as Calcium Oxalate.
2) May be it was not possible to separate all the calcium precipitate from the filter
paper.
3) As the color change was confusing, the end point of titration of KMnO4 with
Na2C2O4, might not have been properly determined.

9 Standardization of Potassium Permanganate solution with Standard Sodium

Oxalate Solution.

Objective: —
The objective of this experiment is to determine the strength of Potassium Permanganate with a
standard Sodium Oxalate solution. This reaction helps to study about oxidation and reduction theory.
As, the color of potassium permanganate changes with the reaction, no further indicator is used in this
experiment to determine the end point.
Theory: —
In this experiment, potassium permanganate solution is standardizing with the help of standard sodium
oxalate solution. The reaction that occurs here is oxidation and reduction reaction. An oxidation-
reduction reaction (redox) is a reaction in which electrons are transferred between species or in which
atoms change oxidation numbers. Oxidation is the half reaction in which there is loss of electrons by
a species (or increase of oxidation number of an atom). Reduction is the half reaction in which there is
a gain of electrons by a species (or decrease of oxidation number of an atom).
Reaction involved in this reaction is:
MnO4- + 8 H + + 5 e- → Mn +2 + 4 H2O
2 KMnO4 + 5 Na2C2O4 + 8 H2SO4 → K2SO4 + 2 MnSO4 + 5 Na2SO4 + 10 CO2 + 8 H2O

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INDICATOR AND WHY USED:
The direct reaction is slow as one can see in a titration. The first few drops of permanganate added
to the acidified oxalate solution are not decolorized immediately. Mn+2 ions produced in the
reaction acts as a catalyst. They react with permanganate to form intermediate oxidation states of
manganese. These states, in turn, react rapidly with oxalate to give the products. So KMnO4 acts
as an auto catalyst in this reaction. This is the advantage of KMnO4 is that it serves as its own
indicator, the pink colour being distinguishable even if the solution is very dilute. Therefore, no
indicator is used in this reaction.

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Apparatus: — Name of the chemicals used: —

1. Conical flask 1.Sodium Oxalate Solution (Na2C2O4)

2.Burette 2.H2SO4 solution (2M)
3.Pipette 3.Potassium Permanganate Solution (KMnO4)
4.Volumetric flask 4. Distilled water
5.Stand
6.Funnel

Procedure:
Prepare 100 ml 0.025M sodium oxalate solution in a volumetric flask. Pipette out 10 mL oxalate
solution in a conical flask. Add about 60 ml 2 M sulfuric acid solutions to it. Add 90-95% of the
required amount of the standard potassium permanganate solution from a burette at a rate of about
25-35 ml/min while stirring slowly. Heat the solution up to 55-600C and complete the titration
quickly by adding permanganate solution until a permanent faint
Data: —
Table1: Data for titration of KMnO4 solution with 0.025M standard sodium oxalate
solution

No. of Volume Burette reading (mL) Volume of Average

Obs. of KMnO4 Volume of
Na2C2O4 Initial Final (mL) KMnO4
(mL) Reading Reading (mL)
(mL) (mL)

Calculation: —
Preparation of sodium oxalate solution:
Molecular weight of C2O4Na2= 134 g/mol
Molarity M= no. of moles (n)/ Volume in L
Amount in g (x)= ?
Or,
1000ml 1M C2O4Na2 = 134
1ml 1M C2O4Na2 = 134/1000
100ml 0.02M C2O4Na2 = (134 ×100×0.02)/ 1000

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 Data for titration of KMnO4 by standard C2O4Na:

Volume of MnO4- taken per titration =10ml

Concentration of C2O42- = [Volume taken/Volume should be taken]*
0.025M= M Volume of C2O42-- = L
Amount of sodium oxalate = volume × concentration
1 mole of MnO4-= 2.5 mole sodium oxalate
Concentration of MnO4- present in solution= (amount of oxalic acid /2.5× volume of
MnO4-)
= mol/L

Result: —
The Determined Strength of Potassium Permanganate Solution is SKMnO4 = M

Precautions: —
At first the burette was cleaned with distilled water carefully; then it was rinsed with
rinse solution to avoid the density change of the given solution. In the same way the
pipette was also washed with distilled water and rinsed with the rinse solution.
a. All the apparatus were handled carefully and according to the rules.
b. The pipette was kept on a clean sheet of paper.
c. The key of the burette was operated carefully to make sure that one-drop of Acid
falls into the conical flask at a time.
d. The conical flask was kept on a white paper to trace the color change of the solution.
e. At first the key of the burette was fully opened to let the solution fall free to
make the bubbles go out.
f. On the basis of the result, it was found that the balance is very much sensitive. So,
for this reason the result can be varied. While measuring the lower meniscus of the
burette an error may be happened for the parallax error. So, concentration should be
needed here.

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