Gc ms

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Published on March 9, 2014

Author: subhradippharmacist

Source: slideshare.net

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GC-MS now a days becoming an important hyphenated technique for the identification of unknown natural samples.

A CLOSER LOOK ON GC-MS [GAS CHROMATOGRAPHYMASS SPECTROSCOPY] BY SUBHRADIP ROYCHOWDHURY* & SATARUPA BHATTACHARJEE** *M.PHARM 2ND SEMESTER DEPT. OF PHARM. SC. B.I.T., MESRA-835215 **B.PHARM 8TH SEMESTER GURU NANAK INSTITUTE OF PHARMACEUTICAL SCIENCE & TECHNOLOGY, KOLKATA

GC-MS – A BRIEF • It’s a Hyphenated Technique • Gas Chromatography + Mass Spectroscopy • Invented By James & Martin in 1952

GAS CHROMATOGRAPHY PRINCIPLES • May be Gas Liquid [GLC] or Gas Solid Chromatography [GSC] but GLC is preferred • GLC works by partition but GSC works by adsorption • In GLC the substance to be studied first converted to gas which works as the mobile phase

MASS SPECTROSCOPY PRINCIPLES 1. Ion Formation 2. Ion Detection & Separation

ION FORMATION • Techniques used to form ions are: 1. Electron Ionisation 2. Chemical Ionisation 3. Desorption Ionisation i. Secondary Ion Mass Spectroscopy [SIMS] ii. Fast Atom Bombardment [FAB] iii. Matrix Associated Laser Desorption Ionisation [MALDI] 4. Electrospray Ionisation

ION SEPARATION AND DETECTION 4 types of instruments are used: i. Direct Focusing Type: a) Single Focusing b) Double Focusing ii. Quadruple Mass Analyser iii. Quadruple Mass Storage iv. Time Of Flight Mass Analyser

INSTRUMENTATION OF GAS CHROMATOGRAPHY A. CARRIER GAS: • Chemically inert • Suitable for the detector use • Amount of impurity should be less • Easily available and should be cheap • Non inflammable Generally used carrier gases are He, H, N, Ar etc.

B. FLOW REGULATORS: Used to maintain the uniform pressure and flow rate Generally used are: • Rotameter • Soap Bubble Flow Meter

C. INJECTION DEVICES: • GAS: Valve Devices • LIQUID: Loop Devices • SOLID: Dissolve the substance in suitable solvent and then inject.

D. COLOUMNS: Columns can be of the following types: • Packed Columns [Stationary Phase- PEG] • Open Tubular Column or Open Capillary Column/ GOLAY Coloumn • SCOT ( Support Coated Open Tubular Column)

E. TEMPERATURE CONTROLLING DEVICES: The devices are very important role playing. Generally used Temperature Controlling Devices are: • PRE HEATERS (For Vapour Formation) • THERMOSTATICALLY CONTROLLED OVEN

INSTRUMENTATION OF MASS SPECTROMETRY PART Consists of: • IONIZATION CHAMBERS • MASS ANALYSERS • DETECTORS

PRINCIPLE OF WORKING AND INTERFACES GC-MS works by 1. ISO THERMAL PRINCIPLE 2. LINER PRINCIPLE Interfaces of GC MS are 1. Molecular Separator 2. Permeation Separator 3. Open Split 4. Capillary Direct

APPLICATIONS • Fire investigation • Drug analysis • Explosive analysis • Environmental analysis • Drug Abuse Analysis

REFERENCE • Silverstein R; Spectroscopic Identification Of Organic Compounds; Wiley Publication Delhi; 6th Edition; 2009; Page 2-70 • Skoog D et al; Fundamentals of Analytical Chemistry; Cengage Brain Publication London; 9th Edition; 2010; Page 16-25 • Kemp W; Organic Spectroscopy; Palgrave Macmillan Limited London UK; 1991; Page 72-75 • mtweb.mtsu.edu/nchong/MS%20Ion%20Sources-Ryan-6200.ppt cited on 11.02.2014

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