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Title:Quality assurance of Aspirin tablets on the basis of

assay of Acetyl salicylic acid and limit of salicylic
acid.
Apparatus required:
i)Conical flasks(250ml),ii)Pipettes,iii)Burettes,iii)Nesslers cylinder(50ml), iv)volumetric flasks(500ml),
v)Graduated pipettes(2ml &10ml).
Chemicals required:
i)Sodium carbonate(AR),ii)0.5MHydrochloric acid(V.S.), iii)0.5M sodium hydroxide, iv)Methyl red
Sol.
n
,v)Phenol red sol
n
, vi)Acid ferric ammonium sulphate solution(IP), vii)Ethanol (95%), viii)Salicylic acid(AR)
Theory:
Acetyl salicylic acid is liable to be contaminated with salicylic acid which may be present as a result of incomplete
conversion to aspirin during manufacture or through hydrolysis on storage.,resulting product are salicylic acid and
acetic acid. So that odour of acetic acid in hydrolysed acetyl salicylic acid is common .
In bulk drug and dosage form of acetyl salicylic acid limit test for salicylic acid should be conducted, the result of
which validates the assay value of acetyl salicylic acid.
Limit test of salicylic acid can be conducted by acidimetry-alkalimetry, HPLC, visual colour comparison method
or colourimetry etc. Assay of acetyl salicylic acid also conducted by acidimetry-alkalimetry, bromometry, UV/Vis
spectrophotometry, HPLC etc.
In limit test of salicylic acid, the calculated amount of acetyl salicylic acid or sample is treated with acidic ferric
ammonium sulphate solution(or with ferric chloride) which reacts with free phenolic group, the violet colour thus
produced should not be more intense than the violet colour produced by the stated amount of salicylic acid
prepared in the same way.
In assay of acetyl salicylic acid, a weighed amount of sample powder is hydrolysed with a measured volume of
excess 0.5M sodium hydroxide. The excess amount of the 0.5M sodium hydroxide is back- titrated with 0.5M
hydrochloric acid(V.S). The final neutralized solution contains sodium acetate and monosodium salicylate.
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The calculation is based on the following relationship

1000ml 1M sodium hydroxide = 1/2 C
9
H
8
O
4
(acetyl salicylic acid) = 180.2/2g.
or,1ml of 0.5M sodium hydroxide = 180.2/4g =0.04504g of acetyl salicylic acid
Procedure:
Wt. of 20 tablets = Avg. Wt. of a tablet=

i)Preparation of acid ferric ammonium sulphate solution:

Dissolve 0.2 g of ferric ammonium sulphate in 50 ml of water,add 6 ml of dilute nitric acid(10%w/w) and add
sufficient water to produce 100 ml.

ii)Preparation and standardization of 0.5M hydrochloric acid:

Dilute 22.3 ml of hvdrochloric acid with water to produce 500m l. Standardise the solution in the following
manner. Weigh accurately about 0.75 g of anhydrous sodium carbonate, previously heated at about 270

C for 1
hour. Dissolve it in 100 ml of water and add 0.l ml of methyl red solution. Add the acid slowly from a burette. with
constant stirring, until the solution becomes faintly pink. Heat the solution to boiling, cool and continue the
titration.. Heat again to boiling and titrate further as necessary until the faint pink colour is no longer affected by
continued boiling. 1 ml of 0.5 M hydrochloric acid is equivalent to 0.0265 g of Na
2
CO
3
.

0.1M hydrochloric acid with (f) = Wt. of Na
2
CO
3 .
=
0.0265g X Vol. of HCl
ii)Limit test for salicylic acid(0.3percent):
Shake a quantity of the powdered tablets containing 0.2 g of Aspirin with 4 ml of ethanol (95 per cent), dilute to
100.0 mi with water, filter immediately, transfer 50 ml of the filtrate to a Nessler cylinder, add 1.0 ml of freshly
prepared acid ferric ammonium sulphate solution, mix and allow to stand for 1 minute; the violet colour
produced is not more intense than that produced by adding 1 ml of freshly prepared acid ferric ammonium
sulphate solution to a mixture of 3.0 ml of a freshly prepared 0.01 per cent w/v solution of salicylic acid, 2 ml of
ethanol( 95 per cent) and sufficient water to produce- 50m l contained in a second Nessler cylinder (0.3 per cent).


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iii)Assay:
Weigh and powder 20 tablets. Weigh accurately a quantity of the powder containing about 0.5 g of Aspirin, add
30.0m l of 0.5M sodium hydroxide,boil gentlyf or l0minutes, cool and titrate the excess of alkali with 0.5 M
hydrochoric acid using phenol red solution as indicator. Repeat the operation w ithout the substance under
examination. T he diff'erence between the titrations represents the amount of sodium hydroxide required.
1 ml of 0.5 M sodium hydroxide is equivalent to 0.04504g of C
9
H
8
O
4
.


Observation:
i)Standardisation:

S.NO Wt. of Initial burette Final burette Total vol. of
titrand(Na
2
CO
3
) reading(ml) reading(ml)
titrant
consumed(ml)
1
2
3


ii) Limit test for salicylic acid(0.3percent):
Complies/Does not comply.

iii)Assay:
S.NO Wt. of Initial burette Final burette Total vol. of
titrand(sample) reading(ml) reading(ml) titrant consumed(ml)
1
2
3
Blank(30ml,
0.5M NaOH)



Calculation:
i)Standardisation of 0.5M hydrochloric acid:
f
1
= Wt. of Na
2
CO
3 .
=
0.0265g X Vol. of HCl
f
2
= Wt. of Na
2
CO
3 .
=
4

0.0265g X Vol. of HCl
Mean (f)=
iii)Assay:
Each table contains aspirin =
1.(Vol. of titrant consumed by blank Vol. of titrant consumed by sample) X f X0.04504g X Avg.Wt. of a tablet
Wt of sample taken(g)
=
2.(Vol. of titrant consumed by blank Vol. of titrant consumed by sample) X f X0.04504g X Avg.Wt. of a tablet
Wt of sample taken(g)
=
Mean=
Result:

Conclusion: