Pharmaceutical Industry – Aspirin Purity

Using back titration to determine the percentage composition of acetylsalicylic acid (2-
acetyloxy benzoic acid) in aspirin

NOTE: A challenge is posed by the fact aspirin is a solid powder which dissolves slowly in
water  Incomplete dissolution would create inaccuracy
 It is therefore necessary to dissolve the aspirin in ethanol (more soluble) and in
excess base to ensure complete dissolution

Back Titration General Outline

1. Aspirin tablet is crushed and added to known volume and concentration of excess
sodium hydroxide in ethanol solvent.
2. After neutralisation is complete, amount of excess sodium hydroxide is found via
titration with standardised hydrochloric acid.
3. Conduct a blank titration of the same known volume and concentration of sodium
hydroxide WITHOUT any aspiring added
4. The moles of base reacted can be calculated by subtracting the excess base from the
total base from the blank  Calculate concentration of ASA
Acetylsalicylic acid is a monoprotic weak acid hence if titration was to be performed, a
strong acid such as NaOH would need to be used to have an identifiable equivalence point.

The difference in titre between the blank and back titration represents the volume of NaOH
required to completely neutralize the ASA in aspirin.
Enrichment: Back Titration
Back titration can be used where direct titration of a sample may be difficult (e.g. sample is a
gas, reaction is slow or incomplete). The titration differs slightly:
1. Add excess reagent to analyte to ensure COMPLETE reaction (shown by excess
addition of B in diagram below)
2. Titrate excess reagent which did not react
3. Calculate moles of excess reagent
4. Subtract moles of excess reagent from total moles of reagent to find amount of
reagent reacted with analyte
5. Calculate moles of analyte reacted stoichiometrically
6. Calculate concentration of analyte
Back Titration Worked Example – 2009 HSC (7 marks)

The nitrogen content of bread was determined using the following procedure:
 A sample of bread weighing 2.80g was analysed
 The nitrogen in the sample was converted into ammonia
 The ammonia was collected in 50.0mL of 0.125M hydrochloric acid. All of the
ammonia was neutralised, leaving an excess of hydrochloric acid
 The excess hydrochloric acid was titrated with 23.30 mL of 0.116M sodium
hydroxide solution
(a) Write balanced equations for the TWO reactions involving hydrochloric acid (2)

(b) Calculate the moles of excess hydrochloric acid (1)

(c) Calculate the moles of ammonia (2)

(d) Calculate the percentage by mass of nitrogen in the bread (2)

SOLUTION: Back Titration Worked Example – 2009 HSC (7 marks)