CLASSICAL METHOD OF QUANTITATIVE

ANALYSIS:

Analysis of H2 SO4
and
H2C2O4 . 2H2O
CHM-657
BS -IV Year
Inorganic Chemistry

Prepared by:

Nabila Hassan
Afshan Suleman
 INTRODUCTION
Chemical
Analysis

Quantitative
Analysis Qualitative
Analysis

Wet Methods Instrumental

methods

Gravimetric Volumetric Optical Separation Electroanalytical

Analysis analysis methods methods methods
 H2SO4
Properties:
It is colorless or slightly yellow viscous liquid.
It is diprotic acid.
It has a dehydrating property.
It is corrosive due to their strong acidic nature.
It is strong oxidizing property.
 Uses:

It is used in Chemical synthesis.

It is used in Fertilizer manufacturing.
It is used in Oil refining.
It is used in Mineral processing.
It is used in Lead-acid batteries.
It is used as Cleaning agent.
It is used as Catalyst.
It is used as Electrolyte.
It is used as Domestic purposes.
 Toxicity and safety:
Laboratory hazards
Industrial hazards
 Analysis:
Analysis Of H2SO4 in a sample solution can be
carried out by Volumetric or Titrimetric Analysis.
It involves acid-base reaction or neutralization
reaction.
 H2C2O4.2H2O

Properties:

It is a colorless crystalline solid.

It is a dicarboxylic acid.
It is a reducing agent.
Its conjugate base Oxalate used as chelating
agents.
It occurs as dihydrate H2C2O4.2H2O.
 Uses:

It is used as bleaching or cleaning agent.

It is used as mordant in dying process.
It is used in Baking powder.
It is an important reagent in Lanthanide Chemistry.
Its reducing properties are used in platinotype (the
early photographic platinum printing process).
It is used to produced shine in marble.
3.2% of oxalic acid solution used in sugar syrup.
 Toxicity and safety:

Oxalic acid has an oral LDLO of 600mg/kg (Human).

Oxalic acid is also a metabolism product of
dehydration of ethylene glycol which is danger for
kidney in case of glycol poisoning as well as
precipitation of calcium oxide.
 Analysis:
Analysis of Oxalic acid in a sample solution can
be carried out by volumetric or titrimetric analysis.
It involves oxidation-reduction reaction or redox
reaction and neutralization reaction as well.
 CHEMICAL REAGENTS:
H2C2O4.2H2O (solid)
NaOH (solid)
KMnO4 (solid)
H2SO4 (dilute solution)
Phenolphthalein (solution)
 PROCEDURE
Standardization of NaOH solution is performed by standard oxalic
acid solution in the presence of Phenolphthalein indicator to
obtained the molarity of NaOH solution.
Total number of mol of H+ produced by sulfuric acid and oxalic
acid can be find out by titrating sample solution by standard
NaOH solution in the presence of phenolphthalein indicator.
Standardization of KMNO4 solution is performed by standard oxalic
acid solution in the presence of sulfuric acid(dilute solution) and heating
at about 700 c to obtained the molarity of KMNO4 solution.
Number of mole of H+ produced by H2C2O4.2H2O can be find out
by titrating sample solution by standard KM NO4 solution in the
presence of H2SO4 (dilute) solution and heating at about 700 c
CHEMICAL EQUATIONS:
Standardization of NaOH Solution Against Standard H 2C2O4 Solution.

Analysis of sample solution.

Reaction of H2C2O4 with NAOH
H2C2O4 + 2NaOH Na2C2O4+2H2O
Reaction of H2SO4 with NaOH
H2SO4 + 2NaOH Na2SO4 + 2H2O
Net Equation (adding Equation 2 & 3)
2NaOH + H2C2O4 + H2SO4
Na2C2O4+ Na2SO4 +4H2O
Reaction of H+ with NaOH
H+ +NaOH Na+ +H2O
Standardization of KMnO4 Solution Against standard
H2C2O4 Solution
Ionization of KMnO4 in Aqueous solution

KMnO4 H2 O4 K + + MnO4
Reduction of MnO4
MnO4 + 8H++5e- Mn+2 + 4H2O
Ionization of H2C2O4 in Aqueous solution

H 2C 2 O 4 H 2O 4 2H + + C2 O4-2
Oxidation of C2 O4-2

C2 O4-2 2CO2 + 2e-

Balancing the number of electrons in equation 7

2MnO4 + 16H++10e- 2Mn+2 + 8H2O

Balancing the number of electrons in equation 9

5C2O4 -2 10CO2+ 10e-

Net equation (adding equations 10 & 11)

2MnO4 + 5C2O4 -2 +16H+ 2Mn+2 + 8H2O + 10CO2
Analysis of sample solution:
Ionization of KMnO4 in Aqueous solution

KMnO4 H2 O4 K+ + MnO4
Reduction of MnO4 -1
MnO4 + 5e-+8H+ Mn+2 + 4H2O
Ionization of H2C2O4 in Aqueous solution

H2 C2 O 4 H 2 O 2H+ + C2 O4-2
Oxidation of C2O4-2
C2O4-2 2CO2 + 2e-
Balancing the number of electrons in equation 14
2MnO4 + 10e-+16H+ 2Mn+2 + 8H2O
Balancing the number of electrons in equation 14
5C2O4-2 10CO2 + 10e-
Net equation (adding equations 17 & 18)
2MnO4 +16H+ + 5C2O4-2 2Mn+2 + 8H2O+10co2
 OBSERVATIONS:

General observations:
i. Total volume of sample solution = 250.0 ml
ii. Weight of H2C2O4.2H2O = 0.6303 g/250.0 ml
iii. Molar mass of H2C2O4.2H2O = 126.0652 g/mol
iv. Weight of NaOH = about 0.4 g/ about 250 ml
v. Molar mass of NaOH = 39.9970 g/mol
vi. Weight of KMNO4 = about 0.2 g/ about 250 ml
vii. Molar mass of KMNO4 = 158.0339 g/mol
viii. Molar mass of H2SO4 = 98.0784 g/mol
 Standardization of NAOH solution:

Volume of standard H2C2O4.2H2O solution=10.0

ml
Indicator = phenolphthalein
Volume of NaOH solution consumed
S No Initial Final Reading Difference Concordant
Reading ml ml Reading
ml ml

1 1.1 10.2 9.1

2 10.2 19.7 9.5 9.5

3 20.1 29.6 9.5

 Determination of volume of standard
NaOH solution consumed against
H2C2O4.2H2O and H2SO4 present in sample
solution.

Volume of sample solution = 10.0 ml

Indicator = Phenolphthalein
Volume of standard NaOH solution consumed
S No Initial reading Final reading Difference ml Concordant
ml ml Reading
ml

01 11.7 21.7 10.0

02 21.7 31.0 9.3 9.3

03 2.3 11.6 9.3

 Standardization of KmnO4
solution:

Volume of standard H2C2O4.2H2O solution=10.0

ml
Volume of dilute H2SO4 = about 10 ml
Volume of KMNO4 solution consumed
S No Initial Final reading Difference ml Concordant
reading ml ml Reading
ml
01 0.4 11.9 11.5
11.5

02 11.9 23.4 11.5

 Determination of volume of standard
KMNO4 solution consumed against
H2C2O4.2H2O and H2SO4 present in
sample solution.

Volume of sample solution = 10.0 ml

Volume of dilute H2So4 = about 10 ml
Volume of standard KMNO4 solution consumed
S No Initial Final reading Difference ml Concordant
reading ml ml Reading
ml
01 8.3 23.9 15.6

02 4.7 19.3 14.6 14.6

03 19.9 34.9 14.6

 CALCULATIONS:

Determination of weight of H2C2O4.2H2O to

present its 0.02M standard solution

Weight of H2C2O4.2H2O = Molarity X Molar mass X volume

1000
Weight of H2C2O4.2H2O = 0.02 X 126.0654 X 250.0
1000

Weight of H2C2O4.2H2O = 0.6303 g/250.0 ml

 Determination of Molarity
of prepared to standard
H2C2O4 solution
Molarity of standard solution = Weight of H2C2O4 X 1000
Molar mass X Volume
Molarity of standard solution = t.abcd X 1000
126.6654 X 250.0

Molarity of standard solution = a.abcd M

 Determination of weight of NaOH
to prepare its 0.04 M standard
solution
Weight of NaOH = Molarity X Molar Mass X Volume
1000
Weight of NaOH = 0.04 x 39.9991 x 250
1000
o Weight of NaOH = about 0.4 g/ about 250 ml
 Standardization of prepared
NaOH solution
1000 ml standard H2C2O4.2H2O solution contains
.abcd mol of H2C2O4.2H2O.
1 ml standard H2C2O4.2H2O solution contains
.abcd/1000 ml of H2C2O4.2H2O.
10.0 ml standard H2C2O4.2H2O solution contains
.abcd X 10.0/1000 mol of H2C2O4.2H2O
= b.abcd mol of H2C2O4.2H2O
1 H2C2O4.2H2O 2NaOH
2 mol of NaOH X b.abcd mol of H2C2O4.2H2O
1 mol of H2C2O4.2H2O
= c.abcd mol of NaOH
 5 ml NaOH solution contains c.abcd mol of NaOH
1 ml NaOH solution contains c.abcd/9.5 mol of
NaOH
1000 ml NaOH solution contains c.abcd X
1000/9.5 mol of NaOH.
d.abcd mol of NaOH

So, the concentration of prepared NaOH solution

is d.abcd M.
 Determination of total no of H+
produced by H2C2O4 and H2SO4 in 250.0
ml sample solution.
1000 ml standard NaOH solution contains d.abcd
mol of NaOh.
1 ml standard NaOH solution contains
d.abcd/1000 mol of NaOH.
9.3 ml standard NaOH solution contains d.abcd X
9.3/1000 mol of NaOH.
= e.abcd mol of NaOH
 1 H+ 1 NaOH
1 mol of H+ X e.abcd mol of NaOH
1 mol of NaOH
= e.abcd mol of H+
10.0 ml sample solution contains e.abcd mol of H+
250.0 ml sample solution contains e.abcd X
250.0/10.0 mol of H+.
= f.abcd mol of H+
 Determination of Molarity of Diluted
standard H2C2O4 solution.
Concentration of prepared standard H2C2O4 c1 = g M
Concentration of diluted standard H2C2O4 c2 = ?
Volume of standard H2C2O4 = V1= 50.0 ml
Volume of diluted standard H2C2O4 : V2; 100.0 ml

C1V1 = C2V2
g X 50.0 = C2 X 100.0
C2 = H.abcd M
So, the concentration of diluted standard of
H2C2O4 solution = H.abcd M
Standardization of prepared KMnO4
solution 1000ml.
1000 standard H2C2O4. 2H2O solution contains H.abcd/mol of
H2C2O4. 2H2O
1ml standard H2C2O4. 2H2O solution contains H.abcd/1000 mol
of H2C2O4. 2H2O
10.0ml standard H2C2O4. 2H2O solution contains
H.abcdx10.0/1000 mol of H2C2O4. 2H2O

2 mol of H2C2O4. 2H2O = 5 H2C2O4 2KMnO4

= j.abcd mol of H2C2O4
11.5 ml KMnO4 solution contains j.abcd mol of KMnO4
1 ml KMnO4 solution contains j.abcd/11.5mol of KMnO4
1000 ml KMnO4 solution contains j.abcdx1000/11.5 mol of
KMnO4
So, the concentration of prepared KMnO4 solution is
K.abcd M
Determination of No of mol of
H2C2O4 .2H2C2O4 present in 250.0 ml sample
solution:

1000 ml standard KMnO4 solution contains K.abcd mol of

KMnO4
1 ml standard KMnO4 solution contains K.abcd/1000 mol of
KMnO4
14.6 ml standard KMnO4 solution contains K.abcdx14.6/1000
mol of KMnO4
= L.abcd mol of KMnO4
5H2C2O4 = KMnO4
5 mol of H2C2O4 x L.abcd mol KMnO4
2 mol KMnO4
= M.abcd mol of H2C2O4
10.0 ml sample solution contains M.abcd mol of H2C2O4
250.0 ml sample solution contains M.abcdx250.0/10.0 mol of H2C2O4
= N.abcd mol of H2C2O4
Determination of weight of H2C2O4. 2H2O
present in 250.0ml sample solution :

Weight of H C O . 2H O = Moles x Molar mass

2 2 4 2

= N.abcd x 126.0654
= O.abcd g/250.0 ml

So, the weight of H C O . 2H O present in 250.0 ml

2 2 4 2

O.abcd g.
Determination of No of mol of H + produced by H SO . present 2 4

in 250.0 ml sample solution.

H C O = 2H+
2 2 4

1 mol of H C O = 2 x O.abcd mol of H+

2 2 4

= P.abcd mol of H+/250.0ml

So, the number of mol of H+ produced by H SO present in 2 4

250.0ml = P.abcd mol

Determination of mol of H+
produced by H2SO4 present in
250.0ml sample solution

No of mol of H+ produced by H2SO4

No of mol of total No of mol of H+ produced

= H+ present in sample - by H2C2O4. 2H2O

solution

= f.abcd - P.abcd
= Q.abcd mol of H+
Determination of No of
mol of H2SO4 present in
250.0 ml sample
solution :
2 H+ = 1 H SO 2 4

1H+ = 1/2 H SO 2 4

Q.abcd mol of H+= mol of H2SO4

= R.abcd mol of H2SO4 /250.0 ml

So, the no of mole of H2SO4 present in 250.0 ml

R.abcd mol
Determination of weight
of H2SO4 present in 250.0
ml sample solution:
Weight of H SO = moles x Molar mass
2 4

Weight of H SO = R.abcd x 98.0784

2 4

Weight of H SO = S.abcd g/250.0 ml

2 4

So, the weight of H SO 2 4 present in 250.0 ml = S.abcd g

Result:-
1. The no of mol of H2C2O4.
2H2O present in the given
sample solution is found to be N.abcd
mol/250.0 ml.
2. The weight of H2C2O4. 2H2O present in the
given sample solution is found to be O.abcd
g/250.0 ml.
3. The weight of H2SO4 present in the given
sample solution is found to be R.abcd
mol/250.0 ml.
4. The weight of H2SO4 present in the given
sample solution is found to be
S.abcd g/250.0 ml.