Spectrophotometric Determination of Aspirin

Experiment 8
The drug with the greatest volume of use is the analgesic, aspirin. The pure
compound (acetylsalicylic acid) with some binder is made into tablets, weighing
slightly less than a third of a gram. When treated with basic solution the
acetylsalicylic acid hydrolyzes quickly to salicylic acid and acetate ions.
O
OH

OCCH3

2 OH-

COH

CO2

acetylsalicylic acid

CH3CO2-

H2O

salicylate
C7H5O3-

The salicylate ions will form an intensely colored complex with the ferric ion in
acidic solution.
3C7H5O3- +
Fe3+
(colorless) (faint yellow)

(C7H5O3)3Fe
(deep red wine)

The wavelength of maximum absorption for this complex is about 530 nm. Thus
visible spectroscopy can be used to measure the amount of aspirin present in the
tablet.

1.

Turn on the spectrometer.

2.

Preparation of unknown. Weigh an aspirin tablet on an analytical balance.

Place it in a clean 50 mL beaker and add 10 mL 0f 0.5 M NaOH. Carefully
crush the tablet with a stirring rod. Dissolve as much of the tablet as possible
and let stand for 10 minutes. Transfer the solution to a 250 mL volumetric
flask being careful to collect all of the solution and rinsings in the flask.

3.

Prepare the following solutions in volumetric flask, diluting to the mark with
water.
A 200 ppm aspirin standard
B 0.1 M Fe3+
C. Unknown

4.

Solution
blk
Std 1
Std 2
Std 3
Std 4
Std 5
Unk

For a 25.00 mL volumetric

A
B
0
4.00
1.00
4.00
2.00
4.00
3.00
4.00
4.00
4.00
5.00
4.00
0
4.00

Solution
blk
Std 1
Std 2
Std 3
Std 4
Std 5
Unk

If you are using a 50.00 mL volumetric

A
B
C
0
8.00
0
2.00
8.00
0
3.00
8.00
0
5.00
8.00
0
8.00
8.00
0
10.00
8.00
0
0
8.00
4.00

Solution
blk
Std 1
Std 2
Std 3
Std 4
Std 5
Unk

If you are using a 100.00 mL volumetric

A
B
C
0
15.00
0
3.00
15.00
0
5.00
15.00
0
10.00
15.00
0
15.00
15.00
0
25.00
15.00
0
0
15.00
5.00

C
0
0
0
0
0
0
2.00

You will team up with a partner and measure all 12 solutions on a

spectrometer. Each of you will use all of the data from you and your partner
in your report. Set the spectrometer at 530 nm, the wavelength of maximum
absorption for the iron salicylate complex. Zero the spectrometer with the
blank. Measure the percent transmittance of each of the standards and the
unknown. It is a good idea to go from dilute to more concentrated and rinse

the test tube in between each measurement. Only touch the top of the test tube
to avoid measurement errors that can occur due to fingerprints. Also, insert
the test tube into the spectrometer in the exact position each time, because
different parts of the glass can scatter light differently and give measurement
errors.
Calculations
1. Convert the % T data to absorbance data
2. Prepare a Beers law plot.
3. From the Least Squares regression, determine the concentration of aspirin in the
final diluted unknown solution.
4. Calculate the percentage (w/w) of aspirin in the tablet.
5. Calculate the error in the concentration obtained in question 3 (see the Guide to
statistics).
6. Propagate errors to estimate the error in the % aspirin calculated in question 4.