3.

1 Preparation and Standardisation of various molar and normal solution of Oxalic Acid :
Oxalic Acid - M.Wt - 126.07
Preparation of 1M Oxalic Acid Solution :
Dissolve an accurately weighed amount of 126.07 gm of Oxalic acid in sufficient amount of water to
give or to produce 1000 ml.
Preparation of 0.1M Oxalic Acid Solution : Dissolve an accurately weighed amount of 12.607 gm
of Oxalic acid in sufficient amount of water to give or to produce 1000 ml.
Preparation of 1N Oxalic Acid Solution :
Dissolve an accurately weighed amount of 63 gm (Since equivalent weight is Molecular wt /No of
replaceable hydrogen ) of Oxalic acid in sufficient amount of water to give or to produce 1000 ml.
Principle : It is an example of alkalimetry. When a strong base is titrated with a weak acid, the salt
produced in the reaction is not completely hydrolysed and the pH of the resultant solution at the
end-point is exactly 7.0 . Oxalic Acid, a weak acid, is standardised by titration with a strong base,
NaOH. The following reaction takes place when NaOH is titrated with Oxalic Acid.
2 ( COOH ) + 2 NaOH →2(COONa) + 2 H2O
In this titration, for detecting the end-point Phenolphthalein solution is used as indicator.
Procedure :
Preparation of 1M NaOH Solution : Dissolve an accurately weighed amount of 40 gm of NaOH
in sufficient amount of water to give or to produce 1000 ml.
Procedure for Standardisation of 1M /1N Oxalic Acid : Take 10 ml of 1M NaOH solution into a
conical flask and add 2 or 3 drops of phenolphthalein indicator. Titrate the contents of the flask
against Oxalic acid solution until the pink colour disappears. Repeat the titration to get concordant
values. Enter the values in a tabular form.
The unknown normality of potassium permanganate is calculated by using the equation
N1V1=N2V2
Where N1 Normality of of Sodium hydroxide
N2 Normality of of Oxalic acid
V1 Volume of Sodium hydroxide
V2 Volume of Oxalic acid consumed
3.2 Preparation and Standardisation of various molar solutions of Sodium Hydroxide
Sodium Hydroxide - M.Wt - 40 ,
Since molecular weight and equivalent weight of sodium hydroxide is same molarity and normality of
sodium hydroxide will be similar.
Preparation of 1M Sodium Hydroxide Solution : Dissolve an accurately weighed amount of 40
gm of Sodium Hydroxide in sufficient amount of water to give or to produce 1000 ml.

Preparation of 0.1M Sodium Hydroxide Solution : Dissolve an accurately weighed amount of

4gm of Sodium Hydroxide in sufficient amount of water to give or to produce 1000 ml.

Preparation of 1N Sodium Hydroxide Solution :

Dissolve an accurately weighed amount of 40gm of Sodium Hydroxide in sufficient amount of water to
give or to produce 1000 ml.

Principle : It is an example of acidimetry. When a weak acid is titrated with a strong base, the salt
produced in the reaction is completely hydrolysed and the pH of the resultant solution at the end point is
more than 7.0 (Alkaline). Sodium hydroxide, a strong base, is standardised by titration with a weak acid,
Oxalic acid.
The following reaction takes place when Oxalic Acid is titrated with NaOH.
2(COOH ) + 2NaOH→ 2(COONa) + 2H2O
In this titration, for detecting the end-point Phenolphthalein solution is used as indicator.
Procedure :
Preparation of 1M Oxalic Acid Solution : Dissolve an accurately weighed amount of 126.07 gm
of Oxalic Acid in sufficient amount of water to give or to produce 1000 ml .
Procedure for Standardisation of 1M Sodium Hydroxide : Take 10 ml of 1M Oxalic Acid solution into
a conical flask and add 2 or 3 drops of phenolphthalein indicator. Titrate the contents of the flask against
Sodium Hydroxide solution until a permanent pink colour is obtained. Repeat the titration to get
concordant values. Enter the values in a tabular form.
N1V1=N2V2
Where N1 Normality of Oxalic acid
N2 Normality of Sodium hydroxide
V1Volume of Oxalic acid
V2Volume of Sodium hydroxide consumed
3.3Preparation and Standardisation of various molar solutions of Hydrochloric
Acid :
Hydrochloric Acid - M.Wt - 36.5
Back ground:
Stock solution of concentrated HCl is around 37% V/V concentration(37 mL in 100 mL)
• Which means it is 370 ml of HCI in 1000ml
Specific gravity of HCl is 1.19g/ml
Density = mass/ volume = 1.19 = X / 370
X = 1.19 * 370= 440.3 g / l
Number of replaceable ions is 1;So molarity = normality
Molecular weight of HCI = 36.5 g;As 36.5 g HCl in 1000ml is1 N
So 440.3 g HCl 1000ml is X N
So normality of the solution stock concentrated bottle is
440.3/36.5= 12.06N or 12N
To prepare the required molar or normal solution
Like 1N from stock 12N
So N1V1 = N2V2
We want = what we have
1 X 1000 = 12 X x
x = 1000/12
= 83.3ml HCl

Preparation of 1M Hydrochloric Acid Solution : Dissolve an accurately measured volume of 83.3

ml of Hydrochloric Acid in sufficient amount of water to give or to produce 1000 ml.

Standardization of 1M Hydrochloric Acid Solution :

It is an example of alkalimetry. When a strong acid is titrated with a strong base, the salt produced in the
reaction is not hydrolysed and therefore the pH of the resultant solution at the end point is 7.0.
The following reaction takes place when sodium carbonate is titrated with HCl.
Na2CO3 + 2 HCl → 2NaCl + H2O + CO2
In this reaction, for the detection of the end-point methyl orange is used as indicator.
Procedure:1.5g of anhydrous sodium carbonate weighed accurately previously heated at about 270˚Ϲ for
1 hour. Dissolve it in mixture of 100 ml of water and add 0.1ml of methyl red indicator solution. Add acid
slowly from burette with constant stirring until solution becomes pink.Heat the solution to boiling cool
and continue the titration. Heat again to boiling and titrate further as necessary until the faint pink color is
no longer affected by continued boiling.

Normality of HCl solution = Weight of AS2O3 X Reqd. Normality

Volume of Ceric ammonium sulphate X Equivalent weight factor
 3.4 Preparation and Standardisation of various molar solutions of Sulphuric acid

Stock solution of concentrated sulphuric acid is around 98% concentration

Which means it is 980 ml of H2SO4 in 1000ml
Specific gravity is 1.835 g/ml
Density = mass/ volume
1.835 = X / 980
X = 1.835 * 980
= 1798.3 g / l
Number of replaceable ions is 2
So 2 molarity = 1 normality or N = M/2
Molecular weight of H2SO4 = 98.08 g
Equivalent weight = 49.04g
As 49.04 g in 1000ml is 1 N : So 1798.3 g in 1000ml X N
So normality of the solution stock concentrated bottle is
1798.3 / 49.04= 36.67 N or 37N
To prepare the required molar or normal solution ,
So N1V1 = N2V2
We want = what we have
1 X 1000 = 37 x X , x = 1000/ 37= 27.03 ml
27.03 ml to be added in 1000ml to get 1N solution of H2SO4

Preparation & Standardization of 0.1 N Sulphuric acid

Preparation : Sulphuric acid is a diprotic acid and 1 N solution contain 98.08/2 = 49.04 g H2SO4.
Taking into consideration specific gravity (1.83) of sulphuric acid about 27 ml of conc. Sulphuric acid is
required to prepare 1000 ml solution.
Theory Standarization is an example of acidimetry. When a strong acid is titrated with a strong base, the
salt produced in the reaction is not hydrolysed and therefore the pH of the resultant solution at the end
point is exactly 7.0. sulphuric acid is a strong acid, is standardized by titrating with a strong base i.e.
sodium carbonate (primary standard). The following reaction takes place when sodium carbonate is
titrated with sulphuric acid. In this titration, end point detection is carried out by using methyl orange
indicator.

Na2CO3 + H2SO4 ==> Na2SO4 + H2O + CO2

procedure –
• 10 ml of 0.1 N Sodium carbonate solution was pipette out into a clean and dried conical flask.
• 2 drops of methyl orange indicator was added to it.
• The contents of the flask were now titrated with sulphuric acid until red colour was obtained.
• Burette reading was taken and tabulated strength of Sulphuric acid is calculated.
3.5 Preparation & Standardization of Various molar solution of Sodium Thiosulpahte
Na2S2O3·5H2O
• Sodium thiosulphate pentahydrate is used
• Molecular weight = 248.17g
• Equivalent weight = 248.17/1 = 248.17
So to get 1N solution we have to take equivalent weight in 1000ml of solvent
Preparation of I N or I M solution of Sodium Thiosulphate
  Take about 100 ml of water in a cleaned and dried 1000 ml volumetric flask.
 Add about 25 gm of Sodium Thiosulphate with continuous stirring.
 Add about 0.2 gm of Sodium Carbonate with stirring.
 Add more about 700 ml of water, mix.
 Make up the volume 1000 ml with water.
 Keep the solution for at least 1 hour before standardization.
Water is boiled before using for sterilization purpose as solution may deteriorate due to bacterial action.
Boiling also expels CO2 which if present as carbonic acid may cause hydrolysis and decomposition of
sodium thiosulphate. Sodium carbonate acts as a preservative to prevent the acid catalysed hydrolysis.

Standardization of 0.N sodium thiosulphate:

The principle of standardization of sodium thiosulphate is based on redox iodometric titration with
primary standards like .
 potassium bromate
 Potassium dichromate
 Potassium Iodate
Potassium bromate is a strong oxidizing agent, it is treated with excess potassium iodide in acidic media
which liberates iodine which is back titrated with sodium thiosulphate.

Potassium iodate is also strong oxidizing agent, it is treated with excess potassium iodide in acidic media
which liberates iodine which is back titrated with sodium thiosulphate.
starch solution is used as indicator.
KIO3+ 5KI + 3H2SO4→ 3K2SO4+3I2+3H2O+ I2
3I2+2Na2S2O3→ 2NaI + Na2S4O6
(Sodium Tetrathionate)
Preparation of 0.1N Sodium thiosulphate
Dissolve 24.8g of sodium thiosulphate pentahydrate(Na2S2O3.5H2O) in 800 ml of freshly
boiled and cooled water and mix thoroughly by shaking for approximately 15 minutes. Make
up the volume to 1000 ml.
Preparation of 0.1N Potassium Iodate: Weigh accurately about 356 mg of KIO3 and dissolve in 100 ml
distilled water
Preparation of Starch indicator : Take 1 gm of soluble starch and triturate with 5 ml of water and add it
to 100 ml of Boiling water containing 10 mg of Mercuric iodide with continuous stirring
Standardisation of 0.1N sodium thiosulphate: Take 10 ml of Potassium Iodate solution .Add 2 gm of
Potassium Iodide and 5 ml of dilute H2SO4,keep it in dark for 10 minutes, add 2 to 3 drops of starch
indicator and titrate with sodium thiosulphte using starch solution as indicator until the blue colour is
disappeared.
Enter the values in a tabular form.
Unknown concentration is calculated using the equation:N1V1=N2V2

3.6 Preparation & Standardization of Ceric Ammonium Sulphate

Molecular weight of ceric ammonium sulphate is 632.5g. Molecular weight and equivalent weight are
same, Molarity of ceric ammonium sulphate = Normality of ceric ammonium sulphate.
Preparation of 0.1 M & 0.1N Ceric ammonium sulphate
Dissolve 65 g of ceric ammonium sulphate with the aid of gentle heat in a mixture of 30 ml of sulphuric
acid and 500ml of water. Cool, filter dilute to 1000ml with water.
Standardization 0f 0.1 M Ceric ammonium sulphate
The standardization of ceric ammonium sulphate can be done by using
1. Arsenic trioxide
2. Ferrous ammonium sulphate
Standardization 0f 0.1 M Ceric ammonium sulphate using Arsenic trioxide
Ceric ammonium sulphate is a strong oxidizing agent standardised by redox titrations (Cerimetric) using
Arsenic trioxide solution as Primary standard in presence of sodium hydroxide, and osmic acid solution
As2O3 + 2NaOH → 2NaAsO2 + H2O
(Sodium Arsenite)
NaAsO2+ 2H2O→ NaH2AsO4+ 2H +4e+
(Sodium Dihydrogen phosphate)
The general expression of cerimetry titration where cerium(IV) reduced to Ce(III)
Ce 4+ + e- → Ce3+
Weigh accurately 0.2g of arsenic trioxide previously dried at 1050 C for 1 hour and transferred to a 500ml
conical flask. Wash the inner walls of the flask with 25 ml of 8%w/v solution of sodium hydroxide
solution. Dissolve the content and add 100 ml of water. Add 30 ml of dilute sulphuric acid , 0.15 ml of
osmic acid, 0.1 ml of ferroin sulphate and titrate with ceric ammonium sulphate until the pink colour
changes to pale blue.
Each ml of ceric ammonium sulphate is equivalent to 0.004946 g of arsenic trioxide
Molarity of ceric ammonium sulphate= Weight of AS2O3 X Reqd. Normality
Volume of Ceric ammonium sulphate X Equivalent weight factor

(ii) Standardization 0f 0.1 M Ceric ammonium sulphate using Ferrous ammonium sulphate
The ceric ammonium sulphate can also be standardized by ferrous ammonium sulphate using ferroin
indicator. At the end point the orange colour of ferrous ammonium colour changes to blue green. During
the reaction ferrous (Fe 2+) oxidised to Ferric (3+)
2FeSO4 (NH4)2SO4.6H2O+2 CeSO4.2(NH4)2SO4.2H2O →CeSO4.2(NH4)2.2H2O+Fe(SO4)3(NH4)2.SO4.6H2O

Oxidation half cell reaction : Fe2+ → Fe3++e-

Reduction half cell reaction : Ce 4+ + e- → Ce3+
Weigh accurately 3.92g of ferrous ammonium sulphate into a conical flask. Add 50ml of dilute sulphuric
acid and make up the volume to 100ml with water. Pipette out 20 ml to a conical flask and titrate against
0.1 M Ceric ammonium sulphate using ferroin as indicator.
The unknown normality of Ceric ammonium sulpahte is calculated by using the equation: M1V 1=M2V2
3.7 Preparation & standardization of Potassium permanganate
Preparation Potassium permanganate solution: The molecular weight of Potasium permanagante is
158 gm. But for the preparation of various normal solution equivalent weight is needed which may differ
according to the medium. (Equivalent weight = Molecular weight/The number of electrons involved in
reaction per mol)
So, in acidic medium 5 electrons are gained, equivalent weight = 158/5 =31.6 g
Acidic medium: The equivalent weight of KMnO4 in an acidic medium is 31.6
Alkaline medium: The equivalent weight of KMnO4 in an alkaline medium is 52.67
Neutral medium: The equivalent weight of KMnO4 in a neutral medium is 52.67 g
Preparation of 0.1 N Potassium permanganate solution
Dissolve 3.2g of potassium permanganate in 1000ml of water, heat on a water bath for 1 hour, allow to
stand for 2 days. Filter the solution through glass wool.
Standardization Of Potassium Permanganate
The principle of standardization of potassium permanganate is based upon redox titration in which
strength of an oxidizing agent is estimated by titrating it with a reducing agent and vice-versa. Potassium
permanganate acts as an strong oxidizing agent in acidic medium that oxidizes oxalic acid in to
carbondioxide. Known strength of oxalic acid is titrated directly with potassium permanganate. End point
can be detected with appearance of permanent pink colour potassium permanganate acts as self indicator

2KMnO4+5H2C2O4+3H2SO4→K2SO4+2MnSO4+8H2O +10CO2
Preparation of 0.1 N Oxalic acid:
6.3 gm of oxalic acid dissolve in 1000 ml of distilled water
Standardisation of 0.1N Potassium permanganate
Take 20 ml of Oxalic acid solution .add 5 ml of 1m sulphuric acid. Warm the mixture to about
70oC .Titrate with potassium permanganate solution taken in the burette. End point is appearance of pink
colour that persist for 30sec.The unknown normality of potassium permanganate is calculated by using
the equation
=N 1V 1=N 2V 2 ;Where N1 Normality of of Oxalic acid
N2 Normality of of Potassium permanganate
V1 Volume of Oxalic acid solution
V2 Volume of Potassium Permanganate consume
Preparation of 1M Potassium permanganate solution
Dissolve 158 g of potassium permanganate in 1000ml of water, heat on a water bath for 1 hour, allow to
stand for 2 days. Filter the solution through glass wool.
Standardization of 1 Molar Potassium permanganate

Take 20 ml of Oxalic acid solution .add 5 ml of 1m sulphuric acid. Warm the mixture to about
70oC.Titrate with potassium permanganate solution taken in the burette. End point is appearance of pink
colour that persist for 30sec
The unknown normality of potassium permanganate is calculated by using the equation: M1V 1=M2V2