Preparation and standardization of

various Molar and Normality

solution

Sem I
Pharmaceutical analysis I
 How to prepare required normality
or molarity solution from available
stock by dilution.
N1V1 = N2V2
(available) = (to be prepared)
Say we have 10N solution and we want to prepare 2N 1
litre from that solution
10*x = 2*1000
X = 2*1000/10
X = 200ml

So we need to take 200ml of stock 10N solution and

dilute it to 1000ml to get the required 2N solution.
Calculation of normality from titration
method using the burette reading

Normality = Weight of the substance x 1000

Burette reading x Equivalent weight x Dilution
factor
 Preparation and standardization of 0.1n oxalic
acid
• (COOH)2 . 2H2O – formula of crystalline oxalic acid
• Molecular weight = 126g
• Equivalent weight = 126/2 = 63g
• So for 1N  63g of oxalic acid dissolved in 1000ml of water 
1N oxalic acid solution
• So for 0.1N  6.3g in 1000ml of water  0.1N oxalic acid
solution
 Preparation of 0.1n oxalic acid

• Weigh 6.3g of oxalic acid in a volumetric flask

• Add water and dissolve it .
• After it has completely dissolved add more water and make
up to the mark to make to 1000ml.
 standardization of 0.1n oxalic acid

• The pure sample of oxalic acid varies due to differences in its

moisture content.
• In this case oxalic acid is heated sufficiently to drive off
absorbed moisture.
• Consequently a solution of approximate concentration is
prepared and its normality is determined against standard
KMnO4 solution.
• Also oxalic acid can be standardized by using NaOH by using
phenolphthalein as an indicator.
standardization of 0.1n oxalic acid with sodium
hydroxide
Prepare 0.5N oxalic acid solution by weighing 3.15g of oxalic acid
and transfer it into 100ml volumetric flask.
Add sufficient amount of water to dissolve then make up the
volume to 100ml
Pipette out 10ml of this solution into conical flask and titrate
against 0.5N NaOH solution using phenolphthalein as indicator
till the end point.
End point is from colorless to pink.
Preparation and standardization of sodium hydroxide
solution

• It is a strong base that is usually used to prepare standard

alkaline solutions useful for volumetric analysis of acidic
compounds.
• It is hygroscopic and reacts with atmospheric CO2.
2NaOH + CO2  Na2CO3 + H20
 Preparation of sodium hydroxide solution

• 40 g of NaOH dissolved in 1000ml of distilled water and

allowed to cool the solution.
• Then the solution saturated with barium hydroxide solution
dropwise with stirring until a precipitate is formed.
• Leave aside for complete precipitation  filter and collect the
filtrate to be standardized against 1N HCl or oxalic acid
Ba(OH)2 + Na2CO3  BaCO3 + 2NaOH
 standardization of sodium hydroxide solution

• 1N HCl is used as a secondary standard.

• 20ml of acid solution was pipetted out and transferred to
conical flask and 50ml of water is added.
• 2 drops of Phenolphthalein was added.
• 1N NaOH solution was taken in a burette.
• Titrate till color changes from colorless to pink.
• Record the volume of 1N NaOH solution used and calculate
the normality.
 Preparation and standardization of
hydrochloric acid solution
• Stock solution of concentrated HCl is around 37%
concentration
• Which means it is 370 ml of HCI in 1000ml
• Specific gravity 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  1000ml  1 N
So 440.3 g  1000ml  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
• 83.3ml to be added in 1000ml to get 1N solution of HCI
• Dilute 83.3ml of conc HCI with distilled water and make up
to 1000ml  1N solution
• 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 .
• Factor calculation
• 1000ml of 1 N HCI  equivalent weight of Na2CO3
• Molecular weight of Na2CO3 = 106g
• Equivalent weight of Na2CO3 = 106/2 = 53g
• Factor = 0.053g
• Each ml of 1N HCI  0.053g of sodium carbonate
• Sodium carbonate contains varying amount of moisture and
sodium bicarbonate
2NaHCO3  Na2CO3 + H2O + CO2
 Preparation and standardization of sulphuric acid
solution

• 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  1000ml  1 N
So 1798.3 g  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
• Like 1N from stock 37 N
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
 standardization of sulphuric acid solution

• 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 color was obtained.
• Burette reading was taken.
• It is an example of alkalimetry.
• When a strong acid is titrated with a strong base, the salt
produced in the reaction is not hydrolyzed 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.
 Preparation and standardization of sodium
thiosulphate solution
• 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
• How to prepare 0.1N sodium thiosulpate solution:
1. Take about 100 ml of water in a cleaned and dried 1000 ml
volumetric flask.
2. Add about 25 gm of Sodium Thiosulphate with continuous
stirring.
3. Add about 0.2 gm of Sodium Carbonate with stirring.
4. Add more about 700 ml of water, mix.
5. Make up the volume 1000 ml with water.
6. Keep the solution for atleast 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
catalyzed hydrolysis.
 Standardization of 0.1n sodium
thiosulphate
• The principle of standardization of sodium thiosulphate is
based on redox iodometric titration with potassium bromate
(primary standard).
• 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 thioslphate.
• Sodium thiosulphate is used in the analysis of iodine.
• In the analysis of iodine starch solution is used as indicator.
 KI + HCI  KCI + HI (hydroiodic acid)
KBrO3 + HI  KIO3 + HBr
KIO3+ 5KI + 6HCI→ 6KCI + 3I2 + 3H2O
I2 + 2Na2S2O3→ 2NaI + Na2S4O6
• Molecular weight of potassium bromate = 167.02g
• Equivalent weight of potassium bromate = 167.02/6 =
27.84g
• Dissolve about g of 2.784g potassium bromate weighed
accurately in sufficient water to produce 100ml.
• To 25ml of the above solution taken in iodine flask, add 1g of
KI and 1.5ml of 2M HCI.
• Stopper the flask immediately and keep in dark for 10mins.
• Titrate the liberated iodine with sodium thiosulphate solution
using starch as the indicator.
• Starch is added towards the end point as indicator until the
blue colour is discharged .
 Preparation and standardization of potassium
permanganate solution
• KMnO4
• Molecular weight = 158.034g
• Equivalent weight = 158.034 / 5 = 31.61g = 32g
• So to get 1N solution we have to take equivalent weight in 1000ml of solvent
 Preparation of potassium
permanganate solution
• Dissolve 3.2 g of reagent grade potassium permanganate
(KmnO4 ) in 1 L of purified water and heat on a steam bath for
two hours.
• Cover and allow to stand for 24 hrs.
• Filter through a fine porosity sintered glass crucible, discarding
the first 25 mL.
• Store in a glass-stoppered, amber-colored bottle.
• Avoid exposure to direct sunlight; cover the neck of the bottle
with a small beaker as a protection against dust.
• If manganese dioxide precipitates on standing, refilter and
restandardize before use.
• Potassium permanganate is an oxidizing agent
• It can retain its conc over a long period under proper storage
conditions and reactions also are rapid.
• Its not a primary standard.
• The ability of KMnO4 solution to oxidize is due to the
conversion of MnO4- to Mn+2 in acidic solution and to MnO4-
2 in alkaline and MnO2 in neutral solution .
• As its not a primary standard it can be standardized by using
sodium oxalate or oxalic acid .
• Sodium oxalate is preferred due to high purity 99.95%sodium
oxalate is dried at 105-110degrees for 2hrs.
• Around 0.67g of pure sodium oxalate is weighed and transferred
to 100ml volumetric flask and solution is made with distilled
water.
• From this take 20ml of solution in conical flask and add 5ml of
conc H2SO4.
• Warm the contents at 70 ˚Ϲ
• Titrate against KMnO4 from burette till faint pink color
persists for 30secs upon shaking the flask.

• 2KMnO4 + 5Na2C2O4 + 8H2SO4  K2SO4 + 2MnSO4 +

8H2O
• Another way is standardization with iodometric method.
• Take 20ml of 0.1N KMnO4 solution , 2g of KI, and 10ml of
H2SO4 was added.
• Titrate the liberated iodine with standard sodium
thiosulphate solution using starch mucilage as the indicator
• Indicator is added towards the end point.

2KMnO4 + 2KI + 4H2SO4  2K2SO4 + 2MnSO4 + I2 + 4H2O

I2 + Na2S2O3  Na2S4O6 (sodium tetrathionate) + NaI
 Assignment

• Preparation of 1N Cerric ammonium sulphate .

• Method of preparation.
• Standardization of the same using sodium oxalate :
Principle, reaction and procedure.
 Preparation and standardization of cerric
ammonium sulphate solution

• 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 if turbid and dilute to 1000ml with water.
• Sulphuric acid is added to avoid precipitation of the basic
salt.
• 0.1N solution
• Ceric ammonium sulphate or Cerium (IV) ammonium sulphate
• Anhydrous form Ce (NH4)4 (SO4)4  596.5 g/mol
• Dihydrate form Ce (NH4)4 (SO4)4 . 2H2O  632.6 g/mol
standardization of cerric ammonium sulphate solution
using sodium oxalate

• Weigh accurately 0.67g of sodium oxalate and dissolve in

water and make up the volume in 100ml volumetric flask.
• Pipette out 10ml of this solution into conical flask and add to
it 15ml dil sulphuric acid and warm the solution to about
70˚Ϲ.
• Titrate this solution against CAS using 2ml of ferroin indicator,
excess drop of CAS reacts with ferroin sulphate and the end
point color is orange red to greenish blue.
• CAS is an oxidising titrant and is not a primary standard.
• Can be standardised using sodium oxalate, arsenic trioxide
oxalic acid etc
• Sodium oxalate in acidic medium acts as an reducing agent
and gets oxidised by CAS .
• Ferroin sulphate acts as indicator which forms complex with
iron.
• At end point colour changes from orange red to greemish
blue.
Na2C2O4 + 2 Ce(SO4)4 (NH4)4  Ce2(SO4)3 + Na2SO4 +
4(NH4)2SO4 + 2CO2
standardization of cerric ammonium sulphate
solution using Arsenic trioxide

• Weigh accurately 0.2g of arsenic trioxide previously dried at

105 ˚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.
• Ceric ammonium sulphate is titrated with Arsenic trioxide
solution (Primary standard) in presence of sodium hydroxide,
and osmic acid solution.
As 2O 3+ 2NaOH → 2NaAsO2+ H2O
NaAsO2+ 2H 2O→ NaH2AsO4+ 2H + + 4e-
Ce 4+ + e- → Ce3