SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC.

SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah
Aim: Preparation of benzanilide from benzophenone
Requirements:
(i) Benzophenone
(ii) Methanol
(iii) Sodium Hydroxide
(iv) Hydroxylamine hydrochloride
(v) Thionyl chloride
(vi) Ether
(vii) Water
Procedure:
Step 1: Preparation of Benzophenone oxime from Benzophenone
Place a mixture of 5.0 g benzophenone and 3.0 g of hydroxylamine hydrochloride and
5.0 mL rectified spirit (methanol) and 1.0 mL of water in the RBF completely dissolve
the substance then add 5.6 g of sodium hydroxide pellets in portion with shaking if
the reaction becomes to vigorous, cool the flask in running tap water attach reflux
condenser and heat it in the water bath for 5-10 minutes (solution should be clear)
then cool it and pour into the mixture of 15 mL HCl and 100.0 mL water white
precipitate of oxime will be separated filter it and wash it recrystallized from
methanol m.p. of product is 142 °C.
Step 2: Preparation of benzanilide from benzophenone oxime
Dissolve 4.0 g benzophenone oxime in 20.0 mL of ether in 100 mL conical flask and
add 3.0 mL of thionyl chloride (the reaction is exothermic) so put Conical flask in the
ice bath or water bath put the flask in the sunlight to remove ether add 25.0 mL of
water and boil for several minutes and break any bumps which may be formed filter
the product, dry it and recrystallized from methanol m.p. of product is 163 °C.
Results:
Step 1: Preparation of Benzophenone oxime from Benzophenone
(i) Theoretical Yield: ______________g.
(ii) Practical Yield: ________________g.
(iii) % Yield of the product: _____________%.
Step 2: Preparation of benzanilide from benzophenone oxime
(i) Theoretical Yield: ______________g.
(ii) Practical Yield: ________________g.
(iii) % Yield of the product: _____________%.

Page | 1
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah
Chemical Reaction:

Mechanism:

Page | 2
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah
Calculation:
Step 1: Preparation of Benzophenone oxime from Benzophenone
(I) Theoretical Yield
Benzophenone: C13H10O (182.0 g.) Benzophenone oxime: C13H11NO (197.0 g.)

From Chemical Reaction

182.0 g. Benzophenone = 197. 0 g. Benzophenone oxime

∴ 5.0 g. Benzophenone = (?) g Benzophenone oxime

5.0 ×197
= = 5.41 g.
182

(II) Practical Yield:

Actual weight of the dried product = ________________g.
𝑃𝑟𝑎𝑐𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 ×100
(III) % of Yield =
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑

= _______________%

Step 2: Preparation of benzanilide from benzophenone oxime

(I) Theoretical Yield
Benzophenone oxime: C13H11NO (197.0 g.) Benzanilide: C13H11NO (197 g.)

From Chemical Reaction

197.0 g. Benzophenone oxime = 197. 0 g. Benzanilide

∴ 5.0 g. Benzophenone = (?) g Benzanilide

5.0 ×197
= = 5.41 g.
182

(II) Practical Yield:

Actual weight of the dried product = ________________g.
𝑃𝑟𝑎𝑐𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 ×100
(III) % of Yield =
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑

= _______________%

Page | 3
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah
Aim: Preparation of 2,4,6 tribromobenzene (symmetrical) from aniline
Requirements:
(i) Aniline
(ii) Glacial acetic acid
(iii) Bromine + Glacial acetic acid
(iv) Alcohol
(v) Sulphuric acid
(vi) Benzene
(vii) Sodium nitrite
Procedure:
Step 1: Preparation of 2,4,6 tribromoaniline from aniline
Dissolve 5.0 mL distil aniline in 19.4 mL gla. Acetic acid shaking well then take 8.6 ml
bromine solution in 20.4 mL gla. Acetic acid in small dropping funnel then add
bromine solution in aniline solution dropwise this reaction exothermic reaction cool
the flask and the final product should be color yellow by adding little more bromine
in cold water and get a product recrystallize in methanol.
Step 2: Preparation of 2,4,6 tribromobenzene (symmetrical) from 2,4,6 tribromoaniline
Dissolve 5.0 g of tri bromo aniline in 15 mL rectified sprite and 3.7 mL of benzene by
heating on a water bath and add 1.5 mL sulphuric acid to the heat solution attach
reflux condenser to the flask and heat on a water bath detach the condenser, remove
the flask from water bath add 1.0 g sodium nitrite shake the flask vigorously allow
the solution to cool for 10 minutes and then immerse the flask in an ice bath a mixture
crystalized out filter with suction on Buchner funnel wash with a small quantity of
alcohol recrystallized the crude from methylated spirit the yield of symmetrical tri
bromo benzene m. p. of 122 °C.
Results:
Step 1: Preparation of 2,4,6 tribromoaniline from aniline
(i) Theoretical Yield: ______________g.
(ii) Practical Yield: ________________g.
(iii) % Yield of the product: _____________%.
Step 2: Preparation of 2,4,6 tribromobenzene (symmetrical) from 2,4,6 tribromoaniline
(i) Theoretical Yield: ______________g.
(ii) Practical Yield: ________________g.
(iii) % Yield of the product: _____________%.

Page | 4
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah
Chemical Reaction:

Mechanism:

Page | 5
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah
Calculation:
Step 1: Preparation of 2,4,6 tribromoaniline from aniline
(I) Theoretical Yield
Aniline: C8H9NO (93 g.) Density = 1.02 g/mL 2,4,6 tribromoaniline: C6H4Br3N (330 g.)

From Chemical Reaction

93 g. Aniline = 315 g. 2,4,6 tribromoaniline

∴ 5.1 g. Aniline = (?) g 2,4,6 tribromoaniline

5.1 ×330
= = 18.1 g.
93

(II) Practical Yield:

Actual weight of the dried product = ________________g.
𝑃𝑟𝑎𝑐𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 ×100
(III) % of Yield =
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑

= _______________%

Step 2: Preparation of 2,4,6 tribromobenzene (symmetrical) from 2,4,6 tribromoaniline

(I) Theoretical Yield
2,4,6 tribromoaniline: C6H4Br3N (330 g.) symmetrical tribromobenzene: C6H3Br3 (315 g.)

From Chemical Reaction

330 g. 2,4,6 tribromoaniline = 315 g. symmetrical tribromobenzene

∴ 5.0 g. 2,4,6 tribromoaniline = (?) g symmetrical tribromobenzene

5.0 ×315
= = 4.77 g.
330

(II) Practical Yield:

Actual weight of the dried product = ________________g.
𝑃𝑟𝑎𝑐𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 ×100
(III) % of Yield =
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑

= _______________%

Page | 6
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah

Aim: Preparation of Eosin from resorcinol or phthalic anhydride

Requirements:
(i) Phthalic anhydride
(ii) Resorcinol
(iii) Zinc chloride
(iv) Bromine
(v) Acetic Acid
Procedure:
Step 1: Preparation of Fluorescein from resorcinol or phthalic anhydride
5.0 g of phthalic anhydride 11.0 g of resorcinol heat the flask in an air bath 180 °C
weight out rapidly 3.5 g of ZnCl2 with string by means of the thermometer mixture
continue the heating at 180 °C at intervals 2-3 minutes until the solutions becomes so
viscous that further stirring is not practicable the result dark red mass consists largely of
a mixture of fluorescein temperature to full to about 90 °C add 100 mL of water and 5 mL
of con. HCl to reaction mixture filter off the insoluble residue of fluorescein of the pump
grind it with water in a mortar and filter again and dry the product.
Step 2: Preparation of Eosin from Fluorescein
5.0 g of fluorescein and 30 mL of spirit in a 150 mL flask make sure that the stopcock
of the funnel is well lubricated before charging the caters with bromine. Add the 8.6 mL
bromine dropwise during about 15 minutes when half the bromine has been converted
into dibromo fluoresceine all the solid material disappears temporarily since dibromo
derivatives is soluble in alcohol further adding to Br2 obtain tetra bromo derivatives.
Results:
Step 1: Preparation of Fluorescein from resorcinol or phthalic anhydride
(i) Theoretical Yield: ______________g.
(ii) Practical Yield: ________________g.
(iii) % Yield of the product: _____________%.
Step 2: Preparation of Eosin from Fluorescein
(i) Theoretical Yield: ______________g.
(ii) Practical Yield: ________________g.
(iii) % Yield of the product: _____________%.

Page | 7
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah

Chemical Reaction:

Mechanism:

Page | 8
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah

Calculation:
Step 1: Preparation of Fluorescein from resorcinol or phthalic anhydride
(I) Theoretical Yield
Phthalic anhydride: C8H4O3 (148.0 g.) Fluorescein: C20H12O5 (332.0 g.)

From Chemical Reaction

148.0 g. Phthalic anhydride = 332.0 g. Fluorescein

∴ 5.0 g. Phthalic anhydride = (?) g. Fluorescein

5.0 ×332.0
= = 11.2 g.
148.0

(II) Practical Yield:

Actual weight of the dried product = ________________g.
𝑃𝑟𝑎𝑐𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 ×100
(III) % of Yield =
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑

= _______________%

Step 2: Preparation of Eosin from Fluorescein

(I) Theoretical Yield
Fluorescein: C20H12O5 (332.0 g.) Eosin: C20H8O5Br4 (648.0 g.)

From Chemical Reaction

332.0 g. Fluorescein = 648.0 g. Eosin

∴ 5.0 g. Fluorescein = (?) g. Eosin

5.0 ×648.0
= = 9.7 g.
332.0

(II) Practical Yield:

Actual weight of the dried product = ________________g.
𝑃𝑟𝑎𝑐𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 ×100
(III) % of Yield =
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑

= _______________%

Page | 9
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah

Aim: Preparation of Benzilic acid from Benzil

Requirements:
(i) Benzil
(ii) Methanol
(iii) Potassium Hydroxide
(iv) Acetic anhydride = 10.0 mL

Procedure:

In your 100 ml round bottom flask containing 24 ml of methanol, dissolve 5.0 g of benzil,
heating the mixture slightly (by means of a heating mantle) if necessary to dissolve the
benzil. Add 16.0 ml of the prepared KOH solution to the reaction flask, while stirring the
contents with your magnetic stir bar. After attaching your condenser to the reaction flask,
reflux the stirred mixture for at least 30 minutes (use a Variac setting of about 40; During
this time, the initial blue-black coloration will change to a brown coloration). Allow the
reaction mixture to cool (remove the heating mantle!), and when the flask is cool enough
to handle, transfer its contents to your evaporating dish. Place the dish on your
stirred/hot plate, and, with low heat, evaporate most of the solvent (this means that when
a layer of solid has formed on the surface of the liquid, stop the evaporation process).
Then, by means of an ice/water bath, cool the dish until the residue solidifies (if this does
not happen in a few minutes, reheat the dish to evaporate more solvent, and repeat the
cooling process). Collect the precipitated solid (crystallized potassium benzilate) upon
your Buchner funnel, and wash it with 2 ml of ice-cold 95% of aq methanol. Next, by
means of your hot plate, dissolve the crude potassium benilate in a minimum amount of
hot water contained in a 250 ml Erlenmeyer flask (NOTE: more than 50 ml of hot water
may be needed to dissolve the solid). Add a small amount of decolorizing carbon to the
flask and stir the hot mixture for a few minutes, then immediately filter the hot solution
by gravity, using two fluted filter papers (one paper inside the other), and collecting the
filtrate in a 250 ml Erlenmeyer flask. Acidify the filtrate by carefully adding 6 ml of
phosphoric acid (NOTE: to assist smooth precipitation of the benzilic acid, occasionally
swirl the Erlenymer flask. Allow the mixture to cool to room temperature (this should
take only a few minutes), then complete the crystallization process by cooling the mixture
in an ice/water bath for five minutes. Collect the precipitated benzilic acid upon your
Buchner funnel, and wash it thoroughly with water to remove any trace of salt present.
13. Then, pace the wet benzilic acid on dry toweling, and allow it to air dry until the next
laboratory period (NOTE: during the next laboratory period after the test but before
checking out, determine the yield and melting point of your purified benzilic acid).

Page | 10
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah

Results:

(i) Theoretical Yield: ______________g.

(ii) Practical Yield: ________________g.
(iii) % yield of the product: _____________%.
(iv) M.P of Benzilic acid: ___________°C

Chemical Reaction:

Mechanism:

Page | 11
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah

Calculation:
(I) Theoretical Yield
Benzil: C14H10O2 (210.0 g.) Benzilic acid: C14H12O3 (228.0 g.)

From Chemical Reaction

110.0 g. Benzil = 218 g. Benzilic acid

∴ 5.0 g. Benzil = (?) g. Benzilic acid

5.0 ×228
= = 5.42 g.
210

(II) Practical Yield:

Actual weight of the dried product = ________________g.
𝑃𝑟𝑎𝑐𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 ×100
(III) % of Yield =
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑

= _______________%

Page | 12
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah

Aim: Preparation of Anthranilic acid from phthalic anhydride.

Requirements:
(i) Phthalic anhydride
(ii) Urea
(iii) NaOH
(iv) Br solution
(v) 10% KOH solution
(vi) Glacial acetic acid
Procedure:

Step 1: Preparation of phthalimide.

Mix phthalic anhydride (10.0 g) and urea (2.0 g) in a 250 ml RBF. Heat the flask on an oil
bath/sand bath/heating mantle at 130-135°C till the content’s melts, froth up and become
solid. Remove the flame and allow cooling. Add water (about 50 ml) to disintegrate the
solid. Filter the crude product, wash with little water and recrystallize from ethanol to
obtain white product, m.p. 230°C, yield about 92%.

Note: Concentrated ammonia solution can be used in place of urea.

Step 2: Preparation of anthranilic acid.

Dissolve 7.5 g NaOH in 40 ml water and cool in ice bath to about 0°C temperature and
then add 2.1 ml Br2 solution to it. To this solution add 5.0 g phthalimide and 20 ml
10% KOH solution, then heat the solution for 5-10 minutes till phthalimide dissolves.
Filter the solution and neutralize the solution with glacial acetic acid. Filter the solid
crystals of anthranilic acid, wash with water and recrystallize from hot water with the
addition of a little decolourising carbon; collect the acid on a Buchner funnel and dry at
100 °C. The pure anthranilic acid, m.p. 145 °C.

Results:

Step 1: Preparation of phthalimide.

(i) Theoretical Yield: ______________g.

(ii) Practical Yield: ________________g.
(iii) % yield of the product: _____________%.
Step 2: Preparation of anthranilic acid.

(i) Theoretical Yield: ______________g.

(ii) Practical Yield: ________________g.
(iii) % yield of the product: _____________%.

Page | 13
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah

Chemical Reaction:

Mechanism:
Step:1

Step:2

Page | 14
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV PRACTICAL
PREPARED BY Dr. Dipen Shah

Calculation:

Step 1: Preparation of phthalimide.

(I) Theoretical Yield

Phthalic anhydride: C8H4O3 (148.0 g.) Phthalimide: C8H5NO2 (147.0 g.)

From Chemical Reaction

148.0 g. Phthalic anhydride = 147 g. Phthalimide

∴ 10.0 g. Phthalic anhydride = (?) g. Phthalimide

10.0 ×147.0
= = 9.9 g.
148.0

(II) Practical Yield:

Actual weight of the dried product = ________________g.
𝑃𝑟𝑎𝑐𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 ×100
(III) % of Yield =
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑

= _______________%

Step 2: Preparation of anthranilic acid.

(I) Theoretical Yield

Phthalimide: C8H5NO2 (147.0 g.) Anthranilic acid: C7H7NO2 (137 g.)

From Chemical Reaction

147.0 g. Phthalimide = 137 g. Anthranilic acid

∴ 6.0 g. Phthalimide = (?) g. Anthranilic acid

6.0 ×137.0
= = 5.6 g.
147.0

(II) Practical Yield:

Actual weight of the dried product = ________________g.
𝑃𝑟𝑎𝑐𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 ×100
(III) % of Yield =
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑

= _______________%

Page | 15
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV
PRACTICAL PREPARED BY Dr. Dipen Shah
Aim: Estimation of Ibuprofen
Principal:
1. The assay of Ibuprofen is carried out by aqueous acid base titration
2. It is weak acid with strong base of neutralization titration.
3. It is based on neutralization reaction of ibuprofen with sodium hydroxide
using phenolphthalein solution as an indicator.
4. Ibuprofen is a iso-butyl-propanoic-phenolic acid. Ibuprofen containing
carboxylic acid react with the NaOH to form the sodium salt of the carboxylic
acid. The salt is typically soluble in water.

Requirement:
1. Beaker 6. Volumetric flask
2. Conical flask 7. Ibuprofen
3. Pipette 8. Sodium Hydroxide
4. Burette 9. Ethanol (95%)
5. Measuring cylinder 10. Phenolphthalein indicator
Theory:
(A) Ibuprofen (Analyte)
a. Molecular Structure

b. Molecular Formula: C13H18O2

c. Molecular Weight: 206.3
d. Chemical Names: (RS)-2-(4-isobutylphenyl) propanoic acid or 2-(4-(2-
methylpropyl) phenyl) propanoic acid
e. Melting Point: 76 °C
f. Description: Ibuprofen is a white, crystalline weakly acid (Ka = 1.2 × 10-5)
solid substrate with slight odour.
g. Solubility: Ibuprofen more soluble in alcohol, very slightly soluble in water.
h. Optical activity: Ibuprofen is chiral molecule so that it exits in two forms (R
and S) s form active in human body
i. Use:
i. Ibuprofen reduces inflammation (non-steroidal anti-inflammatory
drug)
ii. It reduces fever (an antipyretic action) and treats pain (an
analgesic action)
Process: Weigh exactly about 0.4 g of the given Ibuprofen. Dissolve it in 50 mL of
ethanol (95%). Add 2 to 3 drops of phenolphthalein solution as indicator. Titrate this
solution with 0.1 M sodium hydroxide until permanent faint pink color is
developed.
Factor: 1 mL 0.1 M NaOH = 0.02063g ibuprofen
Result: the present purity of given ibuprofen was found to be _____%

Page | 16
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV
PRACTICAL PREPARED BY Dr. Dipen Shah
Calculation:
Reaction:

Observation:
Weight of the given ibuprofen sample = 0.4 g.
Burette : 0.1 M NaOH solution
Flask : Ibuprofen solution
Indicator : Phenolphthalein
End point : Faint pink color developed
Observation Table:
Constant B.R.
No. I.B.R. (mL) F.B.R. (mL) Difference (mL)
A ml
1. 0.0
2. 0.0
3. 0.0

Amount of Ibuprofen

1 mL 0.1 M NaOH = 0.02063g Ibuprofen

X mL y M NaOH = (?)g Ibuprofen

Amount of Ibuprofen = X mL x y X 0.02063

1 X 0.1
= A g.

% Purity of Ibuprofen

For 0.4 g Ibuprofen = 100%

A g Ibuprofen = P%

% Purity of Ibuprofen (p) = A g x 100

0.4
= B %.

Page | 17
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV
PRACTICAL PREPARED BY Dr. Dipen Shah
Aim: To determine the percentage purity of a given sample of Isonicotinic acid
hydrazide tablet.
Principal:
Isonicotinic acid hydrazide/ isoniazid is an anti-tubercular drug. It is assayed by the
direct titration of Potassium bromate with the addition of potassium bromide in the
presence of acid medium using hydrochloric acid. During oxidation reaction
liberated bromine reacts with isoniazid in an aqueous solution to form isonicotinic
acid. Azo dye methyl red indicator is used in this titration, decolorized the red color
is the end point.
Requirement:
1. Conical flask 6. Isoniazid
2. Pipette 7. Hydrochloric acid
3. Burette 8. Potassium Bromide (KBr)
4. Measuring cylinder 9. 0.0167 M KBrO3 solution
5. Volumetric flask 10. Methyl Red Indictor
Theory:
It involves Bromination reaction
Potassium bromate-potassium bromide (KBr-KBrO3) mixture is used for liberation of
bromine.
KBrO3 + 5KBr + 3H2SO4 → 3K2SO4 + 3Br2 + 3H2O
Bromine is then used for bromination of organic compounds.
Excess of Bromine is then determined by addition of KI.
Br2 + KI → I2 + Br-
I2 + S2O3-2 → I- + S4O6-2

Isonicotinic acid hydrazide (Analyte)

a. Molecular Structure

b. Molecular Formula: C6H7N3O

c. Molecular Weight: 137.142
d. Synonyms: Isonicotinic acid hydrazide, Isonicotinyl hydrazine, INHA
e. Solubility: soluble in water.
f. Use:
i. It is an antibiotic used for the treatment for tuberculosis
ii. Also used in the treatment of leprosy in combination with
dapsone

Page | 18
SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV
PRACTICAL PREPARED BY Dr. Dipen Shah
Process:
1. Preparation of 0.0167 M Potassium bromate solution
About 2.784 g of Potassium bromate was dissolved in water and made
up to 1000 ml with distilled water.
2. Assay of Isonicotinic acid hydrazide tablet
Twenty tablets were weighed accurately and pulverized. A weighed quantity of the
tablet power equivalent to 0.25 g INH was transferred into a clean and dry 100 ml
volumetric flask, then sufficient water was added to produce 100 ml. 20 ml of the
above solution was taken. Then 100 ml of water, 20 ml of hydrochloric acid and 0.2
gm of Potassium bromide were added. Then titrated slowly with continuous shaking
with 0.0167M potassium bromate using 0.05ml of methyl red as an indicator until the
red color disappears.
Factor: 1 mL 0.0167 M KBrO3 = 0.003429 g isoniazid
Result: The percentage purity of the given isonicotinic acid Hydrazide tablet was
found to be_____%

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SHRI T. S. PATEL P.G. SCIENCE COLLEGE, AMBALIYARA M.SC. SEM IV
PRACTICAL PREPARED BY Dr. Dipen Shah
Calculation:
Reaction:

Observation:
Weight of the given sample (W) = 0.25 g.
Burette : 0.0167 M KBrO3 solution
Flask : 20 ml of sample + 100 ml of water + 20 ml of HCl and 0.2 g of KBr
Indicator : Methyl Red
End point : red color disappears
Observation Table:
Constant B.R.
No. I.B.R. (mL) F.B.R. (mL) Difference (mL)
A ml
1. 0.0
2. 0.0
3. 0.0

Amount of Ibuprofen

1 mL 0.0167 M KBrO3 = 0.003429 g Isoniazid

X mL 0.0167 M KBrO3 = (?)g Isoniazid

Amount of Ibuprofen = X mL X 0.0003429

1
= A g. (in 20 mL solution)
= A X 5 g (in 100 mL Solution)
= B g (in 100 mL Solution)
% Purity of Isoniazid

For W g Isoniazid = 100%

B g Isoniazid = P%

% Purity of Isoniazid (p) = B g x 100

W
= C %.

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