experiment 5.

2: spectrophotometric analysis of aspIrin

Experiment 5.2: SPECTROPHOTOMETRIC ANALYSIS OF
ASPIRIN

Aim
To find the amount of aspirin in commercial aspirin tablet.

Apparatus Material
 Erlenmeyer flask .0,4033g of acetylsalicylic acid
 Graduated cylinder .10 ml of 1M NaOH
 Volumetric flask . 0,02 M Fe (III)
 Pipet . distilled water
 Weighing scale . half of aspirin (0,2233g)
 Dropper
 spectrophotometer
 Spatula spoon
 Hot plate
 2 cuvettes

Abstract
This experiment utilizes the skills of titration to find the percent mass of actual aspirin
(acetylsalicylic acid) in store-bought aspirin. Two steps and two kinds of titrations
are used. First, approximately 0.1 M NaOH solution was standardized using titration
with KHP. Fe (III) was used because it does not absorb moisture when it is stored,
and it is soluble in water. The reaction that takes place in this reaction is a 1:1 mole
ratio reaction. In part II, we measured five different volumes of ASA solution into 5
test tubes, then filled them up to 50 ml using Fe (III). We had different colours of the
solutions. Found the concentration of the unknown by the calibration curve which
was 0,00144 M.
In the third part, we weighed the aspirin tablet, 0.2233 g then added NaOH and
dissolved it on a hot plate and diluted it in 250 ml volumetric flask with water, took 2,5
ml of that solution to dilute it in 50 ml volumetric flask with iron III. The calculated
mass of acetylsalicylic acid was 0.0072g. This was divided by the initial amount of
aspirin measured (0.2233g) and multiplied by 100 to give the percent mass. This
value is 3.2%. This is not a bad percentage it may be due to that salicylic acid does
not react completely with iron (III) buffer solution.

Introduction
Aspirin is one of the most used pain relievers because of its effectiveness and its
active ingredient, acetylsalicylic acid. Some side effects of aspirin may include
gastrointestinal bleeding and digestive complications if taken in large quantities, so it
is best to take the recommended dosage of aspirin that primary care providers and
pharmaceutical companies suggest. Acetyl salicylic acid (ASA) is one of the oldest
synthetic drugs and widely used medicine. ASA hydrolyses quickly to salicylic acid
and acetate ions when treat with basic solution. The salicylate ions will form an
intensely purple color with the ferric ion in acidic solution. There a spectrophotometer
can be used to measure the amount of aspirin present in the tablet.

This experiment will determine the amount of acetylsalicylic acid (ASA) in a standard
aspirin tablet using spectrophotometric analysis of a solution containing
acetylsalicylic acid and iron (III) ion which forms a purple solution that can determine
the quantification of aspirin through the color intensity using a colorimeter. Using
Beer-Lambert’s Law, which is an equation that states that absorption of light is
independent of its intensity and that the amount of light absorbed is directly related to
the number of molecules of absorbing substance through which the light passes,
absorbance can be determined as 𝐴=𝜖 𝑏 𝐶

Procedure
 1. In a 125 mL Erlenmeyer flask, weigh 0.400g of acetylsalicylic acid. Add
10 mL of a 1 M NaOH solution to the flask and heat to boil.
2. Transfer the solution quantitatively to a 250 mL volumetric flask and
dilute it with distilled water to the mark.
3. Transfer a 2.5 mL sample of this aspirin standard solution to a
volumetric flask of 50 mL. Dilute to the desired concentration with a
0.02 M iron (III) solution. Label this solution "A" and transfer it to a 125
mL Erlenmeyer flask. Run the spectrum of “A” using a
spectrophotometer between 500 nm to 600 nm. Take the reading at 10
nm intervals.
4. Make identical solutions with 2.0, 1.5, 1.0, and 0.5 mL of aspirin
standard. These should be labeled "B, C, D, and E.". measure the
absorbance of each solution at 600 nm.
5. Using a commercial aspirin product, repeat steps 1–3. Brand the
finished solution. Measure the absorbance of the unknown at 600 nm.

Results
Part I: Absorption spectrum of ASA complex

wavelength Absorbance
500 nm 0.708
510 nm 0.710
520 nm 0.709
530 nm 0.698
540 nm 0.681
550 nm 0.658
560 nm 0.630
570 nm 0.598
580 nm 0.562
590 nm 0.522
600 nm 0.481
 1. mass of ASA weighed is 0,4033 g.
molar mass of ASA is 180,2 g/mol.
m 0,4033 g −3
= =2,238 ×1 0 M
n= M g
180 , 2
mol
−3
n 2,238× 10 M
c ASA = =
V 0 , 25 L(250 ml ÷1000)

Diluted c ASA =8,952× 10−5 M

2. graph of absorbance versus wavelength

Absorbance vs wavelength
0.8
0.7
0.6
0.5
Absorbance

0.4
0.3
0.2
0.1
0
480 500 520 540 560 580 600 620
Wavelength

3. The maximum wavelength absorbance of ASA complex is 600 nm

Part II: Construction of a calibration curve

Solution (ml) Concentration (M) Absorbance

0 0 0
2,5 0,0004476 0,508
2,0 0,00035808 0,407
1,5 0,00026856 0,316
1,0 0,00017904 0,188
0,5 0,00008952 0,107

0,0025 L ( 2, 5 ml ÷ 1000 )
c ASA 2 ,5 ml= × ( 8,952 ×1 0−3 M )=0,0004476 M
0 , 05 L ( 50 ml ÷ 1000 )

0,0020 L ( 2 ,0 ml ÷ 1000 )
c ASA 2 ,0 ML= × ( 8,952 ×1 0−3 M )=0,00035808 M
0 , 05 L (50 ml ÷ 1000 )

0,0015 L ( 1 ,5 ml ÷1000 )
c ASA 1, 5 ml= × ( 8,952 ×1 0−3 M ) =0,00026856 M
0 ,05 L ( 50 ml ÷ 1000 )

0,0010 L ( 1 , 0 ml ÷ 1000 )
c ASA 1, 0 ml= × ( 8,952× 1 0−3 M ) =0,00017904 M
0 , 05 L ( 50 ml ÷ 1000 )

0,0005 L ( 0 ,5 ml ÷ 1000 )
c ASA 0 ,5 ml= × ( 8,952 ×1 0−3 M )=0,00008952 M
0 , 05 L ( 50 ml ÷ 1000 )

2. graph of concentration versus absorbance

concentration vs absorbance
0.6

0.5

0.4
absorbance

0.3

0.2

0.1

0
0 0.00001 0.00002 0.00003 0.00004 0.00005
concentration

3 . The Beer-lambert law is a simple linear proportionality between

concentration and absorbance with a formula A=ebc. Therefore, the law is
obeyed since the calibration curve also gives a linear graph. The slope of the
graph of absorbance versus concentration is the extinction coefficient.
Part III: Preparation of unknown from a tablet

Mass of aspirin weigh is 0,2233 g

1. The absorbance is 0,173.

2. The slope of the calibration curve above is
∆ absorbane 0,107−0,508
= =111, 86 . Since the slope of the graph
∆ concentration 0,00008952−0,0004476
of absorbance versus concentration is the extinction coefficient ∴ A=∈ bc
0,173
C unknown= =0,00144 M
1119,861
3. 0,00144 M × 0 ,25 L ( 250 ml ÷ 1000 )=0,00036 g of unknown
0,00036 g
× 0 ,05 L ( 50 ml ÷ 1000 )=0,0072 g of ASA
0,0025 L(2 ,5 ml ÷ 1000)
0 , 0072 g
% mass of ASA¿ × 100
0,2233 g

=3,2% of ASA in the unknown aspirin tablet

Precautions
1.0M NaOH is caustic. Avoid contact with skin, wear gloves and safety glasses at
all times. Be particularly careful when heating the ASA-NaOH mixture on the hot
plate, cover with watch glass to
prevent spattering.

Discussion
In this experiment, spectrophotometric method was applied to analyse aspirin in
commercial aspirin product because this method is common and effective to
complete the analysis. Based on the graph of absorbance of the standards versus
the concentration plotted above, it can be found that the calibration curve is linear. It
shows that the results are agree to Beer-Lambert’s Law. When determining the
concentration (and amount) of acetylsalicylic acid in unknown which was diluted to
different concentration, the calibration curve was used. By calculations, we
determined that the amount of ASA in unknown is 0.0072 g. By using these data, the
percent mass is calculated 3.2%.

Conclusion
We were able to determine the concentration of unknown (0.00144 M) and mass %
of ASA in the aspirin tablet (3.2%). The possible reason for this is personal error
percentage using spectrophotometric analysis. The absorbance of unknown is 0,173
when using the maximum wavelength which 600 nm since it was selected as the
appropriate wavelength.