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NAME:

DATE:
TITLE:
AIM:

THEORY:

are
a
molecule
excess
carried
from
reacted

Marcus Abraham
2nd October, 2016
Back Titration
To determine the percentage of acetyl salicylic acid in aspirin tablets by back
titration with NaOH.
Aspirin, or acetylsalicylic acid (ASA) is a salicylate drug, and is generally
used as an analgesic (something that relieves pain without producing
anesthesia or loss of consciousness) for minor aches and pains, to reduce
fever (an antipyretic), and also as an anti-inflammatory drug. The main
constituent of aspiring is 2-ethanoylhydroxybenzanoic acid (acetyl salicylic
acid, CH3COOC6H4COOH). Aspirin blocks the production of hormones
(chemical messengers formed by the body) called prostaglandins, which are
often released by an injured cell. Prostaglandins in turn trigger the release of
two other hormones that make nerves sensitive to pain. Aspirin's blocking
action prevents this response and therefore is believed to prevent tissue
inflammation. Remarkably, aspirin only acts on cells producing
prostaglandins (for instance, injured cells). The effect of each dose lasts
approximately four hours. Titration is an analytical method involving two
solutions or reactants: an analyte and a titrant. An analyte is of unknown
concentration, while the titrant, also called the standard solution, is of known
quantity. A burette is typically used to carefully add the titrant
to the analyte until a neutral state is achieved. Titration determines an
analyte's strength in terms of molarity, normality, molality, alkalinity, acidity
or precipitatability. Some of the common types of titration methods include
acid-base titration, precipitation titration, reduction-oxidation titration,
complex metric titration and back titration. A back titration is conducted
when one of the solutions is highly volatile such as ammonia; a base or an
acid is an insoluble salt such as calcium carbonate; a reaction is particularly
slow or a direct titration entails a weak base and weak acid titration, the result
of which is hard to ascertain. A back titration is normally done using a twostep procedure. The analyte, which is the volatile substance, is first allowed
to react with the excess reagent. A titration is then performed on the
remaining amount of the known solution to determine how much is in excess
and to measure the quantity consumed by the analyte. Many reactions
slow
or present unfavorable equilibria for direct titration. Aspirin is
weak
acid
that also undergoes slow hydrolysis; i.e., each aspirin
reacts
with
two hydroxide ions. To overcome this problem, a known
amount
of
base is added to the sample solution and an HCl titration is
out
to
determine the amount of unreacted base. This is subtracted
the
initial
amount of base to find the amount of base that actually
with
the
aspirin and hence the quantity of aspirin in the analyte.

MATERIALS
& APPARATUS:

DIAGRAM:

Four (4) aspirin tablets, two (2) 25cm3 pipettes, pipette filler, (8) 250 cm3
conical flasks, 50cm3 burette, retort stand with clamps, white tile, Bunsen
burner, wire gauze, tripod, approx. 1M NaOH, 0.1M HCl, phenolphthalein
indicator, electronic balance, 250cm3 beaker, distilled water in a wash bottle,
two (2) 250cm3 volumetric flasks, glass rod, two (2) funnels.

METHOD:
A) Standardisation of Sodium Hydroxide using 0.1M Hydrochloric Acid
1) 25cm3 of 1M NaOH was pipetted into a 250cm3 standard flask and made up to the
mark with distilled water.
2) 25cm3 of the solution was titrated with 0.1M HCl using phenolphthalein indicator.
3) The titration was repeated until two consecutive values we obtained which differed
by no more than 0.1cm3.
B) Hydrolysis and determination of the quantity of acetyl salicylic acid in aspirin tablets

1) The weight of 1.3 to 1.7g of aspirin was accurately weighed into a 250cm 3
beaker.
2) 25cm3 of 1M NaOH was pipetted followed by25cm3 distilled water on the tablets.
3) The mixture was stirred and simmered gently on a tripod and gauze over a
Bunsen burner for 10 minutes to hydrolyse the tablets (Not to boil)
4) The mixture was cooled and the washings were transferred to a 250cm 3standard
flask. The mark was made up to by distilled water.
5) 25cm3 of the hydrolysed solution was pipetted into a conical flask.
6) Two drops of phenolphthalein were added and the solution was titrated against
0.1M HCl.
7) The titration was repeated till two consecutive values which differed by no more
than 0.01cm3 were obtained.

RESULTS:

Final Volume/cm3
Initial Volume/ cm3
Volume used/ cm3

TABLE 1 SHOWING TITRATION RESULTS FOR TITRATION OF NaOH


AND HCl

Rough
17.80
0.00
17.80

1
36.10
17.80
18.30

2
18.30
0.00
18.30

3
36.40
18.30
18.10

TABLE 2 SHOWING TITRATION TO DETREMINE THE QUANTITY OF


ACETYL SALICYLIC ACID IN ASPIRIN TABLETS

Final Volume/cm3

Rough
4.60

1
9.10

2
13.60

3
18.10

Initial Volume/ cm3


Volume used/ cm3

0.00
4.60

CALCULATIONS:

A)

4.60
4.50

9.10
4.50

13.60
4.50

1) Average volume of HCl used in titration

(18.30+18.30+18.10)
3
=18.23cm3
2) No of Moles of HCl used.
1000cm3 contains 0.1 moles of HCl
18.23cm3

0.1

= 1000 18.23
=1.823 x 10-3 moles

3) Moles ratio
NaOH(aq) + HCl(aq) NaCl(aq) + H2O(l)
It is observed that the mole ration of NaOH: HCl is 1:1
No of Moles of NaOH in 25cm 3= 1.823 x 10-3 moles
4) Actual concentration of NaOH
25cm3 contains1.823 x 10-3 moles
3

1000cm contains

1.823 10
25

1000

Concentration of NaOH= 0.073 mol/dm3

B)

1) Average volume of acid used in titration

(4.5+4.5+4.5)
3
=4.5cm3
2)a) No of moles of NaOH added to the flask before hydrolysis
Average Volume= 4.5 x 10-3 dm3
Concentration of HCl= 0.1M
No. of moles of HCl used
= 4.5 x 10-3 x 0.1
=4.5 x 10-4 moles
NaOH(aq) + HCl(aq) NaCl(aq) + H2O(l)
It is observed that the mole ration of NaOH: HCl is 1:1
No of Moles of NaOH in excess= 4.5 x 10-4 moles
2)b) No of moles of NaOH used in the hydrolysis
No of Moles NaOH at start
= Volume x Concentration
= (0.025) x 0.073
= 1.825 x 10-3 moles
initial moles NaOH -excess NaOH = NaOH used in

hydroylsis
= 1.825 x 10-3 - 4.5 x 10-4 x10
= 1.375 x 10-2 moles
3)

2 Moles of NaOH: 1 Mole of Salicylic Acid


No of Moles of Salicylic Acid= (1.375x 10-2) 2=6.875 x10-3moles
Mass of Salicylic Acid present in aspirin= Moles x Molar Mass
= 6.875 x10-3 x 180.2
= 1.24g
CALCULATIONS:

Therefore the percentage of the tablets that contain salicylic


acid= [ (mass of salicylic acid) (mass of tablets)] x100
=

1.24
100
1.45

=80.5%

DISCUSSION:
ensure

The mixture is simmered gently and carefully during hydrolysis


that the aspirin sample which is a monoprotic acid will completely
dissociated into acetic acid and salicylic acid during the hydrolysis.

It is essential to get all the washings in order to get accurate values


and
not leave any moles behind or left out of the titration. Inactive
ingredients may include hypromellose, powdered cellulose, corn
starch and triacetin. Other possible inactive ingredients in aspirin
tablets include polyethylene glycol, polyvinyl glycol, talc, titanium
dioxide and silicon dioxide. Tablets may also include croscarmellose
dioxide, anhydrous dibasic calcium phosphate and water. The reasons
that could possibly lead to the difference in manufacturers value for
aspirin compared to the obtained value could be the aspirin not being
completely hydrolysed during the hydrolysis process.
SOURCES
OF ERROR:

Improper Weighing of Samples

Faulty lab equipment.


CONCULSION:

The percentage of acetyl salicylic acid in aspirin tablets by back


titration with NaOH was determined to be 80.5%.

REFERENCES:

D.A. Skoog, D.M. West, F.J. Holler and S.R. Crouch, Fundamentals
of Analytical Chemistry, 8th ed. California: Brooks/Cole Thomson
Learning, 2004.
D.C. Harris, Quantitative Chemical Analysis, 7th ed. New York:
W.H.
Freeman and Company, 2010.
R.A. Day, Jr. and A.L. Underwood, Quantitative Analysis, 6th ed.
New Jersey:Prentice-Hall International, Inc., 1991.
Analytical Chemistry Laboratory Manual (2007 Edition). Institute of
Chemistry, University of the Philippines Diliman.