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Principles Of Column Chromatography

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CONTENTS S.No. Topic Page No.
1. About the organization 2. Abstract 3. Introduction 4. Thin layer Chromatography
• Principle of TLC
• Rf value
• Applications and Importance of TLC
5. Column Chromatography
• Stationary phase
• Mobile Phase
• Column
• Conditions for packing the column
6. High Performance Liquid Chromatography
• Principle
• Apparatus
• Uses of HPLC
7. Paroxetine
• Synthesis of Paroxetine.
8. Conclusion. 9. References.

ACKNOWLEDGEMENT

My eight weeks training at the Jubilant Life Science–in API Impurity Management has provided me intensive knowledge and experience of compound isolation techniques.
I have also learnt the systematic functioning, the scientific approach and disciplines maintained …show more content…

The more the compound is soluble, the more it moves up the TLC plate and the less soluble in the mobile phase will stay behind on the TLC plate.
The Rf Value:-
The behavior of an individual compound in TLC is characterized by a quantity known as Rf (Retention Factor).
Rf value = Distance travelled by the compound Distance travelled by the solvent

Fig1. TLC plate showing distances travelled by the compound and the solvent. Applications and Importance of Thin layer chromatography [3]:-
1. Clinical Chemistry, Forensic Chemistry and Biochemistry
2. Cosmetology:-.
3. Food Analysis
4. Environmental Analysis
5. Analysis of Inorganic Substances.

3.3.2 Column Chromatography [5]
It is the method used to separate the impurities present in the sample. It is a type of liquid chromatography as the mobile phase is liquid, the solvent.
 Stationary Phase (Adsorbent):-
The non polar compounds are removed at first position.
The phase where the compound gets adsorbed, mostly Silica is used for this …show more content…

The Wittig reaction is a chemical reaction of an aldehyde or ketone with a triphenylphosphine ylide to give an alkene and triphenylphosphine oxide. Synthesis of Wittig Salt done using 1.334moles triphenyl phosphine and 1.334moles of methlyiodide using toluene as solvent charged in a 5L RB under N2 atm at temperature maintained at 25-30°C and kept overnight. Reaction mixture filtered under vacuum and washed with toluene, dried at 70-75°C for 5-6 hr.
The amount of Wittig Salt obtained =517g.

B) Preparation of DesfluoromethylStyrene.
900ml THF and 0.973moles of Potassium tertiary butoxide, was charged into 5L RB under N2 atm and stirred for 5min 0.936moles of Wittig salt was charged into the above cooled reaction mixture, colour of the reaction mixture changes to yellow. 0.749moles of acetophenone was charged using a dropping funnel and stirred at 30-40○C. TLC checked, it complies, reaction was cooled. Hexane and water charged into it and stirred for 30min at 5-8°C. The reaction mass organic layer was separated followed by its washing with hexane, water and brine, it was filtered under vacuum.
α-Methylstyrene

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