Spectrophotometric Analysis of Commercial Aspirin

Introduction:

Acetyl salicylic acid (ASA) is one of

the oldest synthetic drugs. First
synthesized in Germany by the
Bayer company and marketed
under the name “Aspirin” it has
remained one of the most
popular
“over the counter” drugs of all
time. Its main effect is as a pain
killer and fever depressant, but
in
addition there is strong evidence
that in low daily dosages it lowers
the incidence of heart attacks. In
 Spectrophotometric Analysis of Commercial Aspirin

the last few decades other

drugs such as acetaminophen
(commercial trade name
Panadol, also
Tylenol) and ibuprofen (trade
name Advil) have taken much of
the market for ASA, but ASA
remains
an important and widely used
medicine.
Acetyl salicylic acid (ASA) is one of
the oldest synthetic drugs. First
synthesized in Germany by the
Bayer company and marketed
under the name “Aspirin” it has
 Spectrophotometric Analysis of Commercial Aspirin

remained one of the most

popular
“over the counter” drugs of all
time. Its main effect is as a pain
killer and fever depressant, but
in
addition there is strong evidence
that in low daily dosages it lowers
the incidence of heart attacks. In
the last few decades other
drugs such as acetaminophen
(commercial trade name
Panadol, also
Tylenol) and ibuprofen (trade
name Advil) have taken much of
 Spectrophotometric Analysis of Commercial Aspirin

the market for ASA, but ASA

remains
an important and widely used
medicine.
Acetyl salicylic acid (ASA) is one of
the oldest synthetic drugs. First
synthesized in Germany by the
Bayer company and marketed
under the name “Aspirin” it has
remained one of the most
popular
“over the counter” drugs of all
time. Its main effect is as a pain
killer and fever depressant, but
in
 Spectrophotometric Analysis of Commercial Aspirin

addition there is strong evidence

that in low daily dosages it lowers
the incidence of heart attacks. In
the last few decades other
drugs such as acetaminophen
(commercial trade name
Panadol, also
Tylenol) and ibuprofen (trade
name Advil) have taken much of
the market for ASA, but ASA
remains
an important and widely used
medicine.
 Spectrophotometric Analysis of Commercial Aspirin

Acetyl salicylic acid (ASA) is one of

the oldest synthetic drugs. First
synthesized in Germany by the
Acetyl salicylic acid (ASA) is one of the oldest synthetic drugs. First synthesized in Germany by the
Bayer company and marketed under the name “Aspirin”. It has remained one of the most popular “over
the counter” drugs of all time. Its main effect is as a pain killer and fever depressant, but in addition
there is strong evidence that in low daily dosages it lowers the incidence of heart attacks. In the last few
decades other drugs such as acetaminophen (commercial trade name Panadol, also Tylenol) and
ibuprofen (trade name Advil) have taken much of the market for ASA, but ASA remains an important and
widely used medicine.

Drugs, in addition to their active compound, often contain other inactive ingredients (called
excipients in the pharmaceutical industry) such as binders, fillers, dyes, drying agents, etc. The content
of active ingredient in a tablet will always be stated on the package. In this experiment we will
determine the percent active compound in a commercial aspirin tablet. Aspirin is the trade name for
acetylsalicylic acid (ASA). The ASA in the tablet will be reacted with Fe 3+, forming an intensely violet
colored complex. The concentration of the complex will be determined by means of spectrophotometry,
using a UV/VIS spectrophotometer. Finally, we will be able to calculate the weight and the weight% of
ASA in the commercial tablet.

A colored complex is formed between aspirin and the Fe 3+ ion. The intensity of the color is directly
related to the concentration of aspirin present; therefore, spectrophotometric analysis can be used. A
series of solutions with different aspirin concentrations will be prepared and complexed. The
absorbance of each solution will be measured and a calibration curve will be constructed. Using the
standard curve, the amount of aspirin in a commercial aspirin product can be determined.

The complex is formed by reacting the aspirin with sodium hydroxide to form the salicylate dianion.

O
O C CH3 O- O
(s) + 3OH- (aq) (aq) + CH3C O- (aq) + 2H2O(l)
-
C OH C O
O O

The addition of acidified iron (III) ion produces the violet tetraaquosalicylatroiron (III) complex.
 Spectrophotometric Analysis of Commercial Aspirin

O- O
Fe(H2O)4
+3 +
+ H 2O + H3O
- + [Fe(H 2O)6 ] O
C O C
O O

Methodology:

A. Preparation of the Standard Solutions

1. Using the analytical balance, weigh exactly 0.1600 g ASA in a 50 mL Erlenmeyer flask. Pipet 4 mL of 1
M NaOH solution to the flask, and heat until the contents only begin to boil. Remove from heat
immediately after boiling.

2. Quantitatively transfer the solution to a 100 mL volumetric flask, and dilute with distilled water to the
mark. This is now the aspirin standard stock solution.

3. Using a micropipetor, draw a total of 2.0 mL sample of this aspirin standard solution into a 50 mL
volumetric flask. Dilute to the mark with a 0.02 M iron (III) chloride buffer solution and label this
solution "A".

4. Prepare similar solutions with 1.5, 1.0, 0.5, and 0.1 mL portions of the aspirin standard. Label these
"B, C, D, and E" respectively.

B. Preparation of Unknown sample from tablet

1. Weigh an aspirin tablet in an analytical balance. (The aspirin tablet claims to have 80 mg of ASA)

2. Place the aspirin tablet in a clean 50 mL Erlenmeyer flask. Pipet 10 mL of a 1 M NaOH solution to the
flask, and heat until the contents begin to boil.

3. Quantitatively transfer the solution to a 250 mL volumetric flask, and dilute with distilled water to the
mark.

4. Pipet a 2.0 mL sample of this aspirin tablet solution to a 50 mL volumetric flask. Dilute to the mark
with a 0.02 M iron (III) chloride buffer solution. Label this solution "unknown".

C. Analysis

1. Adjust the wavelength to 530 nm.

2. Insert the blank (cuvette filled with 0.02 M iron (III) chloride buffer solution only) and set 0
absorbance / 100% transmittance.
 Spectrophotometric Analysis of Commercial Aspirin

3. Obtain %T readings for all standard solutions, record. Readings must be done in triplicates.

4. Obtain an absorbance reading for the “unknown” sample.

****ONLY THE WORKSHEET IS TO BE SUMITTED (LAST PART OF THIS DOCUMENT)

 Spectrophotometric Analysis of Commercial Aspirin

Name: PAGKALINAWAN, MICHELLE N. Date: JULY 13, 2020

Instructor: SIR MJ SARNO

Standard Stock Solution:

Weight of Acetylsalicylic Acid (standard) = _____0.1600 g______
Molecular weight of Acetylsalicylic Acid = ____180.2 g/mol____
Diluted to = ______100 mL______
Concentration of standard stock solution (M) = _____0.0089 M_____

Standard solution:

Diluted Am’t of Standard Concentration %T

standard sol’n stock solution(mL) (M)
Trial 1 Trial 2 Trial 3
A 0.1 0.0000178 91.71 90.53 90. 25
B 0.5 0.000089 74.51 74.63 74.58
C 1.0 0.000178 52.01 51.80 52.12
D 1.5 0.000267 36.01 35.81 35.97
E 2.0 0.000356 24.01 24.11 23.93
Aspirin tablet ----------- 7. 42E-05 75.56 76.02 77.03
Volume of diluted standard solutions (mL) = ____50 mL_ ___

Diluted Absorbance Average Standard

standard sol’n Trial 1 Trial 2 Trial 3 Absorbance Deviation
A 0.03758 0.04321 0.04455 0.04178 0.003696
B 0.1278 0.1271 0.1274 0.1274 0.0003501
C 0.2839 0.2857 0.2830 0.2842 0.001357
D 0.4436 0.4460 0.4441 0.4446 0.001273
E 0.6196 0.6178 0.6211 0.6195 0.001651
Aspirin tablet 0.1217 0.1191 0.1133 0.1180 0.004300
**The shaded columns are to be used in the construction of your standard calibration curve

Concentration of Unknown Aspirin: __________7.42E-05 M_________

Milligrams of ASA in tablet sample:____________80 mg__________

%w/w ASA in tablet: ______________________________________

 Spectrophotometric Analysis of Commercial Aspirin

Questions:

1. Explain why 530 nm was the wavelength used for the analysis.

Five hundred thirty nm was the wavelength used for the analysis because the use of the wavelength at
its absorption peak increases the sensitivity of the absorbance measurements.

2. Explain why is there a need for a blank? Why use Fe(III) buffer instead of just water?

Iron (III)Chloride is used as the calibration blank instead of water because in the experiment, we are
calibrating it to the buffer. Before titrant is added, the buffer is absorbing some light so to indicate that
the metal is not having an effect on the solution, the amount of light it absorbs must be measured.

3. How did the amount of aspirin solution compare with the accepted value?

Lambert Beer law states that the absorbance of a light absorbing material is proportional to its
concentration in the solution. This means that the aspirin absorbing light is not equal to its
concentration. As you can see in the table the concentration of aspirin tablet is equal to 7.42E-05 while
the milligrams of ASA in a tablet is equal to 80 mg therefore, they are not equal.

4. Explain how the UV-Vis Spectrophotometer was used to relate absorbance to the concentration of the
aspirin.
Ultraviolet-Visible Spectrophotometer was used to relate absorbance to the concentration of the aspirin
thru calculating both the absorbance and the concentration of the aspirin for us to determine if the
values are equal or not equal.

Schematic Diagram of the Experiment:

 Spectrophotometric Analysis of Commercial Aspirin

0.7 Calibration Curve:

0.6
f(x) = 1728.6 x − 0.01
R² = 0.99
0.5

0.4

0.3 Linear ()

0.2

0.1

0
0 0 0 0 0 0 0 0 0

Calculations:

Concentrations of Standard Stock Sol’n (M):

0.1660/180.2 = 0.000887902

0.000887902/0.100 = 0.0089M

Concentration (M):

M1 V ₁ = M2V2

M₂ = M₁V ₁/ V ₂

(0.0089) (0.1)/50 = 0.0000178

(0.0089) (0.5)/50 = 0.000089

(0.0089) (1.0)/50 = 0.000178

(0.0089) (1.5)/50 = 0.000267

(0.0089) (2.0)/50 = 0.000356

Absorbance:

2-log(%T)

Average Absorbance:

f(x)/n
 Spectrophotometric Analysis of Commercial Aspirin

Linear Equation:

R2 = 0.9948

Slope (m) = 1728.5x

y-intercept = -0.0103

y=mx+b

Concentration of Unknown Aspirin:

y=mx+b

x=y-b/m

0.1180+0.0103
x=
1728.5
x = 7.42E-05

Conclusion: