CHANDIGARH UNIVERSITY

UNIVERSITY INSTITUTE OF PHARMACEUTICAL

SCIENCE
LAB MANUAL

(PHARMACEUTICAL ANALYSIS-I)

PHP-109

B.Pharmacy (1st SEM)

MS. PARMINDER KAUR

ASSISTANT PROFESSOR
E-CODE: 6056
 Pharmaceutical Analysis- I – 1stsem

List of Practicals

CHEMICALS
S.NO NAME OF EXPERIMENT
REQUIRED

1 To study and practice the technique using analytical balance.

2 To study instruments like pipette ,burette and titration flask

used in quantitative analysis

3 To prepare 1M HCl and standardize it and perform assay of HCl,sodium hydrogen

sodium hydrogen carbonate. carbonate, methyl red
indicator

4 To prepare and standardize 0.1M silver nitrate and ammonium Silver nitrate, ammonium
thiocynate and to perform assay of sodium chloride. thiocynate, NaCl,
methanol, acetic acid,
nitric acid

5 To prepare and standardize 1M sodium hydroxide and study NaOH, Boric acid,
the assay of given sample of Boric acid. potassium hydrogen
phthalate,
phenolphthalein,
glycerine

6 To perform and standardize 0.1M sodium thiosulphate and to Sodium thiosulphate,

perform the assay of iodine iodine, KI, HCl, iodine

7 To prepare and standardize 0.02M potassium permanganate KMNO4, H2O2, Sodium

and to perform assay of the given sample of solution of thiosulphate, Sodium
hydrogen peroxide carbonate

8 To determine the water of hydration in crystalline Barium Barium chloride

chloride

9 To determine the %age of chlorine in sodium chloride NaCl, sodium

thisulphate, sulphuric
acid, starch, KMNO4
10 To carry out assay of given sample of sodium chloride Eosin, NaCl, AgNO3,
injection potassium chromate

11 To prepare & standardize 0.1N KMNO4 against oxalic acid KMNO4, oxalic acid,
H2SO4

12 To prepare & standardize 0.1N H2SO4 using sodium carbonate H2SO4, oxalic acid,
Na2CO3, methyl orange
LABORATORY MANUAL

EXPERIMENT NO: 1

AIM: To study and practice the technique using analytical balance.

APPARATUS: Butter paper, spatula, weight box, analytical balance

STEPS FOR USING ANALYTICAL BALANCE:

1. Before using ensures that the balance is placed on a firm platform and both the
pans are clean.
2. Check that the balance is placed perfectly, horizontally as indicated by the
pointer.
3. Switch off the fans before weighing because it will disturb the balance blow
the chemical to be weighed
4. Raise the beam by turning a knob or key clockwise and observe the movement
of pointer. If the beam is not moving to and fro then the analytical balance is
not balanced.
EXPERIMENT No: 2
AIM: To study instruments like pipette, burette and titration flask used in
quantitative analysis.
REQUIREMENTS: Pipette, burette, titration flask, measuring cylinder, glass rod
THEORY:
1. PIPETTE: Normal values of pipette are 1 ml, 2 ml, 5 ml, 10 ml, 20ml. Before
filling any solution, it is rinsed with small amount of same solution. It is then
filled by dipping the tip under liquid and applied suction from mouth to about
1-2 cm above graduation mark. The entire liquid above graduation mark is
allowed to drain in an extra container. After this the remaining liquid in the tip
should not be forced out by blowing or by shaking or by any other way.

2. Micropipettes allow for the repeated and accurate delivery of the same volume.
They come in different sizes, typically dispensed volumes can vary from 5 or
10 microliter (μl) to as much as 5 or 10 ml. Some models have a single fixed
delivery volume, while others have adjustable volumes within a certain range.

3. BURETTE: It is used for titration and consists of a cylindrical tube with a

constricted end to which a narrow glass tube is attached by means of rubber
 tube. There is a spring dip, when this is pressed with two fingers solution is
released from the burette. Burette is graduated in ml, 0 being at the top. Reading
is taken from division corresponding to lower edge of meniscus with the eye on
the same level. Before each titration, liquid level in burette must be adjusted to
‘0’ mark.

4. MEASURING CYLINDER: These are suitable for volume measurement with

precision needed. In volumetric analysis, they are used only for measuring out
various reagents which are not needed for calculation of result.

5. TITRATION FLASK: It is a flask used for carrying out titration. It should have
a wide neck, a big belly and flat bottom. It should be thoroughly washed with
distilled water and not with the sample.
6. GLASS ROD: Mixing or stirring of solution is carried out by means of glass
rod. This is made of glass having diameter of 3-5mm.
7. GLASS FUNNELS are used to fill burettes, larger funnels together with folded
or fluted filter paper are used to filter impurities or product from solutions.

8. BUCHNER FUNNELis used to collect the final product of a laboratory

synthesis process. It is used together with an aspirator that draws a vacuum
thereby pulling the liquid through the filter paper while the pure solid product is
collected on the filter.
EXPERIMENT NO: 3

AIM: To prepare 1M HCl and standardize it and perform assay of sodium

hydrogen carbonate.

APPARATUS: Pipette, burette, glass rod, funnel, dropper, titration flask,

volumetric flask

PROCEDURE:]

PREPRATION OF TITRANT: Measure out 21.25 ml of pure conc. HCl and

transfer it to a 250 ml distilled water in a beaker.

STANDARDIZATION OF HCl: Weigh accurately 1.5g of anhydrous sodium

hydrogen carbonate and dissolve it in 100ml water. Now add 0.1ml of methyl red
as indicator.

Take HCl in a burette. Now prepare the solution of sodium hydrogen carbonate of
1.5g and add 0.2 ml methyl orange as indicator and make the volume of volumetric
flask up to 100ml.After this, with the help of pipette suck 20 ml of solution of
sodium hydrogen carbonate and put into titration flask. Then step by step put HCl
into titration flask and remember to stir continuously the solution. Note the end
point i.e. change of orange to pink colour and also check the reading of the burette
that how much quantity of HCl is used.
EXPERIMENT NO: 4

AIM: To prepare and standardize 0.1M silver nitrate and ammonium thiocynate
and to perform assay of sodium chloride.

APPARATUS: Pipette, burette, Glass rod, weight box, titration flask, volumetric
flask, funnel, spatula.

PROCEDURE:

Take 0.1M of silver nitrate in a burette and mark the initial reading. Now by using
analytical balance weigh 0.1g sodium chloride.Dissolve it in 5ml of water + 5ml of
acetic acid + 50ml of methanol and 0.15ml of eosin solution. Stir it and then titrate
it with0.1M silver nitrate. Pipette out 20mlof 0.1M silver nitrate to titration flask.
Dilute it with 50 ml of water and add 2ml of nitric acid and 2ml ferric ammonium
thiocynate solution. Titrate it with ammonium thiocynate solution, the colour
changes to red brown colour. Note the reading. Again perform the experiment for 2
times and take out the concordant reading. Calculate the %age purity from the
above information.
EXPERIMENT NO: 5

AIM: To prepare and standardize 1M sodium hydroxide and study the assay of
given sample of Boric acid.

APPARATUS: Pipette, micropipette, titration flask, weight box, beaker, funnel,

measuring cylinder, spatula

PROCEDURE:

Take 1M sodium hydroxide in the burette and mark the initial reading. Now weigh
accurately 5g of potassium hydrogen phthalate. Dissolve it in 75ml of water and
then add 0.1ml of phenolphthalein and titrate it with sodium hydroxide till light
pink colour is obtained. Note the reading .Again perform the experiment for 2
times .Take 2 concordant reading .Calculate the morality of given sample of
sodium hydroxide.

Take 25ml of glycerin in titration flask. Add 2 drops of phenolphthalein in it. Then
titrate it with sodium hydroxide till light pink color is obtained. Then add 50 ml of
water in it. Take 500mg boric acid in another titration flask, add the solution in it.
Shake it and 1 drop of phenolphthalein in it .Then titrate it with sodium hydroxide
till permanent pink color is obtained. Take the reading by performing the
experiment 3 times .Calculate the %age purity.
EXPERIMENT NO:6
AIM: To perform and standardize 0.1M sodium thiosulphate and to perform the
assay of iodine.
APPARATUS: Pipette, micropipette, titration flask, Iodine flask, weight box,
beaker, funnel, measuring cylinder, spatula, burette
PROCEDURE:
Prepare 0.1M Sodium thiosulphate solution by dissolving 6.25g of sodium
thiosulphate and 0.05g of potassium carbonate in Carbon dioxide free water and
then make the volume up to 250ml.Transfer it to the burette and note the initial
reading. Now in titration flask take 0.20g of potassium bromated in 250ml of
water and 2g potassium iodide and 3ml of 2M HCl and transfer the ingredients
in iodine flask. Allow the reaction to proceed in dark for 5 minutes. The solution in
iodine flask turns deep red. Now in another titration flask pipette out 20ml of this
solution and titrate it against 0.1M solution taken in burette. When the solution
turns yellowish green, add 2ml of starch solution. The solution turns deep blue.
Then add few drops of 0.1M Sodium thiosulphate and the color disappears. Note
this as final reading.
Perform the experiment 2 times and note the concordant reading. To perform the
assay of iodine weigh 0.2g of iodine and add it in 1g of potassium iodide and 2ml
of water. Again add 250ml of water. Titrate it against 0.1M Sodium thiosulphate
taken in burette in the same way as done with potassium iodide solution. Use
starch solution as indicator. Perform the experiment and note three concordant
readings. Now by taking volume of titrate and morality to calculate %age purity.
EXPERIMENT NO: 7

AIM: To prepare and standardize 0.02M potassium permanganate and to perform

assay of the given sample of solution of hydrogen peroxide.

APPARATUS: Burette, pipette, micropipette, weight box, beaker, titration flask,

funnel, measuring cylinder, spatula

PROCEDURE:

Firstly to prepare 0.02M Potassium permanganate solution, add 0.8g of it in 250ml

water. Heat it for 1 hour and then filter it with glass wool. Allow it to stand for 48
hours to complete the reaction. Cover it with a foil. To standardize the prepared
potassium permanganate, prepare 0.1M Sodium thiosulphate solution. To prepare
this add 6.25g of sodium thiosulphate and 0.05g of sodium carbonate. Now titrate
it against potassium permanganate solution. To prepare the titrate 25ml of
potassium permanganate is taken in stopper flask
EXPERIMENT NO: 8

AIM: To determine the water of hydration in crystalline Barium chloride.

APPARATUS: Fractional weights, sample, china dish, burner or spirit lamp and
desiccators

PROCEDURE:

1. Weigh about 1.3933g of anhydrous Barium chloride previously heated and dry
it in china dish.
2. Place china dish with substance resting on low burner flame at height of 5-6 cm.
3. At the interval of few minutes, china dish may be heated by means of strong
blue flame to dull redness.
4. Heating to dull redness at the end is done continuously for ten minutes.
5. Allow china dish to cool at room temperature and then transfer it to dessicator
for 15 minutes and weigh .Then weigh the sample.
EXPERIMENT NO: 9

AIM: To determine the %age of chlorine in sodium chloride.

APPARATUS: Burette, pipette, measuring cylinder, butter paper, fractional

weights, funnel, glass rod

PROCEDURE:

1. Prepare 0.1M sodium thiosulphate by dissolving 0.8 g of it in 250ml water.

2. To 25ml of potassium permanganate solution taken in a stopper flask, add 2g
potassium iodide and 10 ml of 1M sulphuric acid.
3. Titrate it with 0.1M Sodium thiosulphate using 3ml of starch solution. End
point is disappearance of blue color.
4. Now perform assay of Hydrogen peroxide by adding 1ml of it, 20ml of 1M
sulphuric acid and titrated with 0.02M Potassium permanganate to pink end
point.
EXPERIMENT NO: 10

AIM: To carry out assay of given sample of sodium chloride injection.

PROCEDURE:

PREPARATION OF TITRANT:

To prepare 0.1N silver nitrate i.e., 4.247g of silver nitrate is dissolved in 250ml of
water.

STANDARDISATION OF 0.1N SILVER NITRATE:

Weigh accurately about 0.1g of sodium chloride (previously heated at 110°C for 2
hours) and dissolve it in 5ml water.Add 5ml acetic acid and 50ml methanol and
0.15ml eosin solution.Stir and titrate with 0.1M silver nitrate solution.Take 2-3
concordant readings and find out the exact molarity of the sample.

ASSAY OF SODIUM CHLORIDE INJECTION:

This is carried out by Mohr’s method. Weigh 0.1g of sodium chloride.Add about
50ml water and then titrate it with 0.1N Silver nitrate using potassium chromate as
an indicator. Take 2-3 concordant readings and find out the %age purity of the
sample.
EXPERIMENT NO: 11

AIM: To prepare & standardize 0.1N KMNO4 against oxalic acid.

PROCEDURE:

PREPARATION OF 0.1N OXALIC ACID:

Dissolve 0.63g of oxalic acid in distilled water and make the volume upto 100 ml.

PREPARATION OF 0.1N KMNO4:

Dissolve 3.16g of KMNO4in distilled water and make the volume upto 1000 ml.

STANDARDIZATION

Pipette out 10 ml of oxalic acid into a conical flask. Add 5 ml of conc. Sulphuric
acid to it. Fill the burette with KMNO4 and titrate until a pink color persists.

Calculate the normality of KMNO4 by

N1V1=N2V2
EXPERIMENT NO: 12

AIM: To prepare & standardize 0.1N H2SO4 against sodium carbonate.

PROCEDURE:

PREPARATION OF 0.1N H2SO4:

Dissolve 5.6 ml of H2SO4 in distilled water and make the volume upto 1000 ml.

PREPARATION OF 0.1N Na2CO3:

Dissolve 0.53 g of Na2CO3in distilled water and make the volume upto 100 ml.

STANDARDIZATION

Pipette out 10 ml of Na2CO3 into a conical flask & add 2-3 drops of methyl orange.
Add 5 ml of conc. Sulphuric acid to it. Fill the burette with H2SO4 and titrate until a
point where color changes to orange red color from golden yellow.

Calculate the normality by

N1V1=N2V2