Chemistry Lab Report

Experiment (9): Spectrophotometric analysis of a commercial tablet

1- Aim: To Determine the % active ingredient of a commercial

Aspirin.

2- Introduction:
A colored complex is formed between aspirin and the iron (III) 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 CH 3 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.
+

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

(1)
 3- Apparatus and Chemical:
UV/VIS spectrophotometer and polystyrene
cuvettes Hot plate (4) 15mL test tubes (2)
10mL graduated pipette 5mL graduated pipette
Apparatus
150mL beaker 10mL graduated cylinder 100mL
volumetric flask 50mL volumetric flask watch
glass.
1 commercial aspirin tablet ( 50mL >> 0.000725M
) salicylic acid (reagent grade) ( 50mL >> 0.02M)
Chemical
FeCl3 (buffered to pH = 1.6 with HCl/KCl) 10mL
1.0M NaOH.

4- Discussion:

A) Preparation of the Fe-salicylate standard solutions and the calibration curve:

1. Use a 10 ml graduated pipette to transfer 1.0, 3.5, 6.5, and 9.5 ml
of 0.000725 M salicylic acid solution into four separate test tubes.
Label these solution SA1, SA2, SA3, SA4, respectively.
2. Make the total volume in each test tube equals to 10.0 ml by adding
0.02 M FeCl3 solution using a 10 ml graduated pipette.
3. Measure the absorbance of the four standard solutions at 530 nm
using the cuvette provided. Start with the lowest concentration (solution
SA1). Rinse the cuvette with the next solution (SA2) then measure the
absorbance of this solution, etc.

B) Analysis of the ASA in a commercial aspirin tablet:

(This Procedure can be done at the same time as preparing the standard
solution)
1. Weigh a commercial aspirin tablet directly into 150 ml beaker.
2. Add 3.5 ml of 1 M NaOH (use 10 ml graduated cylinder).
3. Place the beaker on a hot plate at the lowest temperature. Slowly
heat the mixture for about 5 minutes or until all solid is dissolved. Then
allow the solution to cool and the undissolved material to settle down.
4. Decant the liquid solution into a 100 ml volumetric flask and fill to
the mark with distilled water. Label this solution "STOCK ASA
UNKOWN".
5. Transfer 1 ml of Stock ASA UNKOWN solution (with a 5 ml
graduated pipette) to 25 ml volumetric flask. Fill the flask to the mark

(2)
with 0.02 M FeCl3 solution. Label this solution "ASA UNKNOWN" The
presence of binders and fillers in the tablet may make the solution
cloudy, but this will disappear when diluted with the acidified Fe +3
solution.
6. Measure the absorbance of the ASA UNKOWN solution at 530 nm.

5- Results & Calculation:

(A) Standard solution and Beers law calibration curve:

1- Fill in the following table:
Solution Absorbance Concentration, M
SA1 0.141 0.0000725
SA2 0.526 0.000254
SA3 0.861 0.000471
SA4 1.199 0.000689

2- Make a graph of Absorbance vs. Concentration C (mol/L):

(3)
(B) Analysis of unknown aspirin tablet:
1- Mass of aspirin tablet = 0.3571 g
2- Absorbance of ASA UNKNOWN = 0.166
3- Concentration of ASA UNKNOWN as determined from the calibration
curve,
CASA UNKNOWN = 0.0000953 g/mol
4- Concentration of STOCK ASA UNKNOWN,
CSTOCK ASA UNKNOWN = (50/1.0)*CASA UNKNOWN = 50 * 0.0000953 =
0.004765 g/mol
5- Moles of ASA in 100mL solution = 0.1* 0.004765 = 0.0004765 mol
6- Mass of ASA = mol*molar mass = 0.0004765 * 180 = 0.08577 g
7- % of ASA in aspirin = (0.08577/0.3571)*100 = 24.02 %

6- Conclusion: We learn from this experiment how to determine

the % active ingredient of a commercial Aspirin by using
Spectrophotometric analysis. And we find in this experiment that the
active ingredient of a commercial Aspirin is 24.02 %.

(4)