EXPERIMENT 3: Determination of Aspirin Tablet in an Ultraviolet region of the EMR

spectrum

COURSE NAME AND CODE: ANALYTICAL CHEMISTRY 2A ACH260S

SEMESTER AND YEAR: SEMESTER 1, 2023

GROUP NUMBER: B2

STUDENTS IN GROUP: ALANDE MFEKETHO

MGUBE MESULI

MJIKWA ZINGAPHI

MKHIZE SANELISIWE

STUDENT NUMBERS: 222013362

222171782

221441379

221383670

SUBMISSION DATE: 17 APRIL 2023

PLAGIARISM DECLARATION:

We Alande Mfeketho (222013362), Mgube Mesuli (221441379), Zingaphi Mjikwa,

(222171782), Sanelisiwe Mkhize (221383670), declare that the work we submit is our
own. We understand that if, for any reason, we are suspected of copying or plagiarising, we
will follow the protocols needed. If found guilty we will be penalized and adhere to the
disciplinary guidelines and procedures applicable.

Signature:
Aim

This is to determine the acetylsalicylic acid content in a commercial aspirin tablet by UV-VIS
spectroscopy analysis. The aim of determining the number of aspirin in a commercial tablet is to
determine the concentration of an active ingredient in the tablet and verify that it meets the labeled
potency. This information is important for quality control and consumer safety, as variations in the
number of active ingredients can significantly impact the product's effectiveness and safety. The
determination process involves analyzing the tablet for its aspirin content using various analytical
methods and comparing the results with established standards and specifications.

Introduction

Acetylsalicylic acid is an energetic ingredient in the most widely used non-prescription drug. When the
aspirin is ingested, acetylsalicylic acid is hydrolyzed in the stomach into salicylic acid which serves as an
analgesic antipyretic. It showcases antipyretic house through suppressing the manufacturing of
carboxyhemoglobin that inhibits the biosynthesis of prostaglandin and produces analgesia by using
virtue of each peripheral CN effect (Witch et.al 2023) salicylic acid work by inhibiting extraordinary
chemical natural and herbal acne inflammation. The distinct strength of aspirin tablets is structured on
the range of acetylsalicylic acid present. Aspirin is positive in the elevation of headache and joint pain.

THEORY

The determination of aspirin in a commercial tablet can be conducted using various analytical methods
such as high-performance liquid chromatography (HPLC), gas chromatography (GC), spectrophotometry,
and titration.

A sample of the tablet is dissolved in a suitable solvent and injected into the chromatographic apparatus
in the HPLC procedure. Aspirin is extracted from the column and detected using a UV detector at a
particular wavelength using an appropriate mobile phase. By comparing the peak area of the injected
sample to that of a standard aspirin solution, the quantity of aspirin in the sample is then calculated. The
preferred method for aspirin analysis in commercial tablets is the HPLC method since it is both very
accurate and sensitive.
A sample of the tablet is dissolved in an appropriate solvent and inserted into the chromatographic
apparatus in the GC technique. A capillary column is then used to isolate the aspirin from the other
components in the sample before it is discovered using a flame ionization detector. The peak area of the
injected sample is then compared to that of a reference aspirin solution to determine the concentration
of aspirin in the sample. While the GC method is more accurate and sensitive than HPLC, it also requires
more time for analysis.

The spectrophotometric approach uses aspirin's absorption of light at a certain wavelength to

determine its presence. A sample of the tablet is dissolved in a suitable solvent, and a
spectrophotometer is used to gauge the solution's absorbance. A calibration curve built from standard
aspirin solutions with known concentrations is then used to calculate the aspirin concentration in the
solution. A spectrophotometric method is straightforward and affordable, however, it is less sensitive
than HPLC and GC techniques. There are various analytical techniques that can be used to determine the
amount of aspirin in a commercial tablet. The spectrophotometric and titration procedures are less
complex and more affordable substitutes for HPLC, which is the most accurate and sensitive approach.
The approach selected relies on the equipment's accessibility, and the desired sensitivity the most
precise and sensitive approach is HPLC, whereas the simpler and less expensive spectrophotometric and
titration methods are alternatives. The method chosen will rely on the equipment that is available, the
level of sensitivity needed, and the complexity of the sample matrix.

Procedure

Part A

A spectrometer was set up to scan a spectrum. The spectrometer was zero using air as a reference.
When running the scans of cuvettes, cuvettes were cleaned and scans were run separately using air as a
reference, and print out of each cell were obtained The dilatated stock solution was given in a 25 cm3
volumetric flask which was benzene (AR) in heptane (AR), 5:25 (v/v) if the benzene solution with
heptane (AR) was diluted. The spectrometer was set up to scan spectra with water as a reference. A
correct set of cuvettes was chosen for the analysis, water was used as a reference. The instrument was
made zero and the baseline was recorded.

Part B

Stock solution A was prepared by weighing 0.1g of salicylic acid and was transferred to a 100 ml
volumetric flask. 1 ml of NaOH was added and filled up the mark with distilled water. Five separate
100ml of the volumetric flask were used. 10ml, 20ml, 30ml, 40ml, and 50ml were pipetted and 1ml of
NaOH was added to each of the flasks and they were filled up to the mark with distilled water. 3 ml of
diluted salicylic acid was used to obtain the absorption spectrum. The absorbance of each standard at
maximum wavelength was measured.

Part C

Two aspirin were given, and they were accurately weighed. The masses were found to be 0,4646g and 0,
4712g. Pestle and mortar were used. Tablets were crushed separately. The powder was transferred into
two separate 100ml beakers and 20ml of NaOH was added to dissolve the aspirin. The solution was
filtered into a 250ml volumetric flask, it was topped to the mark 0.1M of NaOH and shaken for about 2
minutes. 2ml of the liquor was pipetted into a 100ml volumetric flask and filled up to mark with distilled
water. The absorbance of the solution at the same wavelength for the standards was measured. The
calibration curve was used to determine the concentration of salicylic acid in each aspirin solution. The
weight of salicylic acid present in the aspirin by considering dilutions was involved.

Results

Preparation of standards

Mass weighed of salicylic acid= 0, 0984

salicylic acid = m/M

= 0,0984g/(138,12gmol)

=7,124×10-4M/0.1

=7,124×10-3mol/L ×138.12g.mol× 1000

=983.41mg/L

Dilution of salicylic acid

For 1ml

CiVi = CfVf

(983.41mg/L) (1ml) = Cf(100ml)

983.41/100 = Cf

9.83mg/L = Cf

For 2ml

CiVi = CfVf

(983.41mg/L) (2ml) =Cf(100ml)

1966.82/100 = Cf

19.67mg/L = Cf

For 3ml

CiVi = CfVf

(983.41mg/L) (3ml) = Cf(100ml)

2950.23/100 = Cf

29.50mg/L = Cf

For 4ml

CiVi = CfVf
(983.41mg/L) (4ml) = Cf(100ml)

3933.64/100 = Cf

39.33mg/L = Cf

For 5ml

CiVi = CfVf

(983.41mg/L) (5ml) = Cf(100ml)

4917.05/100 = Cf

49.17mg/L = Cf

The maximum wavelength of salicylic acid was 295 nm.

Table 1

The below shows salicylic acid dilutions with their absorbance.

Standards Volume(ml) Concentration(mg/L) Absorbance

1 100 9.83 0.6483
2 100 19.67 0.8914
3 100 29.50 1.1196
4 100 39.33 1.3701
5 100 49.17 1.8914

The calibration curve shows the relationship between the concentration and absorbance of salicylic acid.
 Absorbance vs Concentration
2

1.8
f(x) = 0.0301365639054519 x + 0.299131364789169
1.6 R² = 0.9668940047872

1.4

1.2
Absorbance(au)

0.8

0.6

0.4

0.2

0
5 10 15 20 25 30 35 40 45 50 55

Concentration(mg/L)

Determination of acetylsalicylic acid in commercial tablet

Table2

Determination of absorbance of the two 100ml solutions 295nm

Sample Volume Absorbance

1 100 0.2967
2 100 0.2607

Y= (0.0301x) + (0.2991)

0.2967= (0.0301x) +(0.2991)

0.0024/0.0301=x

18.16mg/L= x
{SA}= Concentration of SA x Molar of ASA/molar mass of SA

= (18.16mg/L) (180.16g/mol)(1)/138.12g/mol

= 23.68mg/L/1000

=0.02368g/L

Weight of acetylsalicylic acid

0.02368g/L= m/(180.16g.mol) (0.1L)

m=0.4266g

Percentage error

% error= True value – experimented value/ True value

%error= 0.4646g- 0.4266g/0.4646g×100

%error= 8.17%

Sample2

Y= (0.0162x) +(0.0024)

0.2607= (0.0301x) + (0.2991)

0.2583/0.0301=x

15.94mg/L=x

{SA}= concentration of SA× Molar SAA/ mass of SA

= (15.94mg/L) (180.16g/mol) ×1/138.12g/mol

=20.79mg/L/1000

= 0.02079g/L

Weight of acetylsalicylic acid

0.02079g/L = m(180.16g/mol) (0.1L)

M= 0.3745g

Percentage Error
%error = true value – experimented value/ true value×100

%error = 0.4712g- 0.3745g/0.4712g×100

%error= 20.52%

Discussion
In part 1 we measured five different volumes of salicylic acid solution and filled it with NaOH. We had a
colored solution (chromophore). We used a quart cuvette and UV spectrophotometer to measure
absorbance. Plastic and glass cuvette has more absorption compared to quartz cuvette, which is why we
used quartz cuvette. The calibration curve is linear (straight line), so it agrees with beer law as it
represents the linear relationship between absorbance (A) and concentration (c). The calculate
concentration of salicylic acid is 983.41mg/L.

In part, a calibration curve with a straight line was drawn with a concentration of the five standards
9.83mg/L to 49.17mg/L of aspirin. The equation of the calibration is obtained that was y= (0.0301x)
+(0.2291). As the concentration increases more radiation is absorbed and the absorbance increases as
well, and the concentration is directly proportional to the absorbance. The percentage errors were
calculated and were found to be 8.17% and 20.52%.

Conclusion

The concentration of salicylic acid was 0.02368g, the weight of acetylsalicylic acid was 0.4266g and the
percentage error was 8.17%. The other salicylic acid concentration was 0.02027g/L, the weight of
acetylsalicylic acid was 0.3745g and the percentage error was 20.52%..the determination of aspirin in a
commercial tablet can be conducted using several analytical methods. HPLC is the most accurate and
sensitive method, while the spectrophotometric and titration methods are simpler and cost-effective
alternatives. The choice of method depends on the availability of equipment, the required sensitivity,
and the complexity of the sample matrix.

APPENDIX

Preparation of standards

Mass weighed of salicylic acid= 0, 0984

salicylic acid = m/M

= 0,0984g/(138,12gmol)

=7,124×10-4M/0.1

=7,124×10-3mol/L ×138.12g.mol× 1000

=983.41mg/L

Dilution of salicylic acid

For 1ml

CiVi = CfVf

(983.41mg/L) (1ml) = Cf(100ml)

983.41/100 = Cf

9.83mg/L = Cf

For 2ml

CiVi = CfVf

(983.41mg/L) (2ml) =Cf(100ml)

1966.82/100 = Cf

19.67mg/L = Cf

For 3ml

CiVi = CfVf

(983.41mg/L) (3ml) = Cf(100ml)

2950.23/100 = Cf

29.50mg/L = Cf

For 4ml

CiVi = CfVf

(983.41mg/L) (4ml) = Cf(100ml)

3933.64/100 = Cf

39.33mg/L = Cf

For 5ml

CiVi = CfVf

(983.41mg/L) (5ml) = Cf(100ml)

4917.05/100 = Cf

49.17mg/L = Cf

The maximum wavelength of salicylic acid was 295 nm.

References
1. Salah, M. Abubaker, M. L. and Kamal, E. E. I. (2005). J. Flow injection Anal,
22(2), 118-122.
2. Veeresh, T. M., Lamani, S. D. and Nandibewoor, S. T. (2009). Mechanistic and
spectroscopic investigations of oxidative degradation of aspirin by aqueous
alkaline permanganate. Transition metal chemistry,317-324.
3. https://www.academia.edu/36388927/
exeriment3spectrophotometric_ANALYSIS_OF_ASPIRIN