Determination ASPIRIN in some pharmaceutical products by using Spectroscopic A Dissertation By : Muna A. Abdulla Supervised By :

Dr. Hamad M. IdrissDr. Abdulrazeq

OverviewPart 1. Introduction

Part 2. Preparation Standard

Part 3. Making an Unknown for a tablet

Part 4. Melting Point Measuring

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Overview

Part 5. SpectroPhotometric

Part 6. Results and Tables

Part I. Introduction• In this experiment you will learn how to use a chemical reaction to make

new substances such as aspirin:Salicylic acid + Acetic anhydride Aspirin + Acetic acid

• The complex ion is formed in two steps. First the acetylsalicylic acid is reacted with sodium hydroxide to form the salicylate dianion. Then the addition of acidified iron (III) ion produces the violet tetraaquosalicylatroiron (III) complex.

• The UV spectrophotometric\ analyses are often preferred in quality control testing and ordinary laboratories due to its broad availability and suitability.

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Part II. Preparation Standard

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100 mg salicylic acid Add 10 ml NaOH solution

Mass 400 mg of acetylsalicylic acid in a 125 mL Erlenmeyer flask. Add 10 mL of a 1 M NaOH solution to the flask, and heat until the contents begin to boil.

Part II. Preparation Standard

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

Part II. Preparation Standard• Pipet a 2.5 mL sample of this aspirin standard

solution to a 50 mL volumetric flask. Dilute to the mark with a 0.02 M iron (III) solution. Label this solution "A," and place it in a 125 mL Erlenmeyer flask.

• 4. Prepare similar solutions with 2.0, 1.5, 1.0, and 0.5 mL portions of the aspirin standard. Label these "B, C, D, and E."

Part III. Making an Unknown for a tablet

One ASPIRIN tablet NaOH solution

Place one aspirin tablet in a 125 mL Erlenmeyer flask. Add 10 mL of a 1 M NaOH solution to the flask, and heat until the contents begin to boil.

Part III. Preparation an Unknown from a tablet

• Quantitatively transfer the solution to a 250 mL volumetric flask, and dilute with distilled water to the mark pipet a 2.5 mL sample of this aspirin tablet

solution to a 50 mL volumetric flask. Dilute to the mark with a 0.02 M iron (III) solution. Label this solution "unknown," and place it in a 125 mL Erlenmeyer flask.

Part IV. Melting Point Measuring

• Materials:

melting point tube

melting point apparatus

Spectrophotometer

Results• Fig I: Standard curve of ASPIRIN

Results• Table I: Show the

absorbance of commercial ASPIRIN sampleCommercial aspirin Absorbance

Aspar aspirin 0.75

Aspocid 0.71

Asprine 1.2

Aggrex 1.3

Results• Table II: show the concentration by ppm of commercial

ASPIRIN sample

• Commercial aspirin Concentration ppm • Aspar aspirin 78.12ppm• Aspocid 72.44ppm• Asprine 132.29ppm• Aggrex 144.79ppm

Results• Table III: show weights by gram of commercial

ASPIRIN sample

• Commercial aspirin Weight • Aspar aspirin 0.15g• Aspocid 0.14g• Asprine 0.16g• Aggrex 0.19g

Results • Table IV: show melting point of standard and

commercial ASPIRIN sample

• Commercial aspirin Weight • Standard aspirin 136 ◦c• Aspar aspirin • Aspocid 125 ◦c • Aspirin 102◦c • Aggrex 166 ◦c

Conclusion • This analytical method also used in ordinary

Laboratories, It can also be adopted for quality control tests for the drugs which contain aspirin in tablets, the obtained results by using UV-Vis spectrometer indicated that , there is some different in aspirin contents between the calculated values and the the real concentrations . Also there is different in the melting point between the standard samples and the measured ones .

Thank You For Listen