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By: alkurdii (17 month(s) ago)

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By: alkurdii (17 month(s) ago)

this is grat thank you guys

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Slide 1: 

By Chandra sekhar Hemanth Kranthi basha M PHARMACY 1ST YEAR DEPT.OF PHARMACEUTICAL ANALYSIS SWAMI VIVEKANANDHA COLLEGE OF PHARMACY

Slide 2: 

Introduction Amines are two types 1. Aliphatic amines 2. Aromatic amines Aliphatic amines: Primary alkyl amines( methylamine, ethanolamine) Secondary alkyl amines (dimethyl amine) Tertiary amines (triethyl amine ) Cyclic amines(piperidine) Aromatic amines: aniline, trimethy aniline…. etc

DETERMINATION OF AMINES : 

DETERMINATION OF AMINES General methods 1.Acetylation (acid base titration) 2.Bromination (iodometric titration) 3.Non aqueous 4.Picrate method

Slide 4: 

Acetylation method: Principle: (CH₃ CO)₂ + H₂O 2CH₃COOH CH₃COOH + NaoH CH₃COONa+H₂O

Slide 5: 

Reagents used : Acetic anhydride in pyridine: Acetic anhydride (1vol)+ pure dry pyridine (3vol) Mixed indicatior: 0.1% aqueous cresol red (one part)+0.1% aqueous thymol blue(3 parts) Alcoholic NaoH solution (0.5M): 20gm NaoH + 1000ml ethanol or methanol.

Slide 6: 

Procedure: 2 milli-equivalents sample +6ml acetic anhydride ↓ Shake gently and cool ↓ Add 10ml water ↓ Again shake and cool ↓ Add 10ml butanol+mixed indicator ↓ Titrate with 0.5M alcholic NaoH solution ↓ End point is blue colour Perfom blank titration also

Slide 7: 

Formula: (V₁- V₂) X MX molecular weight X 100 weight of sample X 1000 V₁= blank NaoH soln value V₂= NaoH soln used for sample M= molarity of NaoH %NH₂ =

Slide 8: 

Bromination method : Principle: KBrO3 +5KBr +6HCl 3Br2 + 6KCl +3 H2O Br₂ + KI 2 KBr + I₂ I₂ +Na₂S₂O₃ 2NaI + Na₂S₄O₆

Slide 9: 

Reagents used: Potasium bromate and bromide solution: 5.567gmKBro₃ +75gm gm KBr + HCl + H₂O sodium thio sulphate : 25gm Na₂S₂O₃ + 1litre water Starch indicator: 1gm starch +100ml boiling water +3gm KI KI solution: 100gm KI +400ml water

Slide 10: 

Procedure: 0.25gm sample +min volume dil Hcl ↓ Make upto 250ml with distilled water ↓ Pipette out 25ml soln +25ml bromate bromide soln+25ml water+5ml conc Hcl ↓ Shake vigourously and cool ↓ Add 10ml 20%KI soln ↓ Again shake vigourously + water + starch indicator ↓ Titrate with free I₂ with 0.1M Na₂S₂O₃ ↓ End point is blue colour

Slide 11: 

Perform blank titration. Formula: (V₁-V₂)X strength of titrant X M.Wt of sampleX100 wt taken X 2000 X No of Br₂ substituted V₁= blank titrevalue V₂= sample titre value % NH₂=

Slide 12: 

Nonaqueous method Reagents used: Acetous Perchloric acid: 8.5ml 72% perchloric acid+500ml glacial acetic acid +20ml acetic anhydride Methyl violet: 30mg methyl violet +100ml chlorobenzene Crystal violet: 1gm crystal violet +100 ml glacial acetic acid

Slide 13: 

CH3COOH CH3COOH + H+ HClO4 H+ + ClO4- CH3COOH + H+ CH3COOH2 CH3COOH2+ + CH3COO- 2CH3COOH PRINCIPLE:

Slide 14: 

Procedure: 0.3gm of amine + 50ml glacial acetic acid ↓ Add crystal violet indicator or methyl violet ↓ Titrate with perchloric acid ↓ End point is blue green or green Perform the blank titration also

Slide 15: 

Formula : (V₁- V₂)X MX M.wt X 100 W X 1000 V = blank titre value V= sample titre value M= molarity of perchloric acid M= molecular weight amine W= weight of sample % NH2=

Slide 16: 

Picrate method Reagents used: 1.Crystal violet indicator 2.acetous perchloric acid PICRATE REACTION

Slide 17: 

Formula: wt of picrate of amine X 1000 Vol of acetous perchloric acid X N Procedure: 0.8gm picrate of amine +50ml glacial acetic acid + Add crystal violet indicator ↓ Titrate with 0.1M acetous perchloric acid ↓ End point is blue green colour Eq.Wt =

Slide 18: 

References: Quatitative organic analysis IInd edition By Arthur Vogel Page no: 697-705 Pharmaceutical titrimetric analysis by A.A Napoleon Wikepedia

Slide 19: 

thank you