Gas chromatography

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  • Split injection :dipakaikalosampelkadarnyatinggi, splitlessdipakaikalosampelkadarnyarendahbangetdanbutuhdipekatkandikit, on column kalosampelmudahrusakpadasuhutinggi
  • Gas chromatography

    1. 1. Gas Chromatography Compiled by : Imanuelle Orchidea 3325102413
    2. 2. Definition • A chromatographic technique in which the mobile phase is a gas Gas Gas –Liquid/ Gas-Solid Chromatography Liquid Solid
    3. 3. Rangkaian penghubung & penguat Tabung gas perekam
    4. 4. Mobile phase • Inert gas ( He, Ar, N2) • Carry the sample • Flow rates determined with a flow meter placed at a column outlet Column type Flow rate Packed column 25-150 mL/min Capillary column 1-25 mL/min
    5. 5. Packed columns Capillary columns
    6. 6. Packed Columns – Glass/stainless steel/copper/aluminum – 2-6 m in length, internal Ø 2-4mm – Particle Ø ranging from 37-44 µm to 250-354 µm – diatomaceous earth, glass beads, fluorocarbons polymers – Handle larger samples – Pressure needed to move mobile phase limits it’s length
    7. 7. Capillary Columns • Open tubular column – Wall-coated – Support-coated • Fused silica coated with protective polymer • Up to 100 m in length • Internal Ø 150-300 µm, megabore up to 530 µm • Handle smaller samples ( < 10-2 µL)
    8. 8. • Photo of capillary column, taken from Harvey, David .T. Modern Analytical Chemistry
    9. 9. Stationary phase • Choice of stat. phase  selectivity • Criteria : – CHEMICALLY INERT – THERMALLY STABLE – LOW VOLATILITY – APPROPRIATE POLARITY • R – SiR2 – O - (SiR2 – O)n – SiR3 • HO – CH2 – CH2 – (O – CH2 – CH2)n – OH
    10. 10. STAT.PHASE POLARITY TRADE NAME (T)LIMIT APPLICATIONS Squalane Non-polar Squalane 150 Low boiling aliphatic hydrocarbons Apezion L Non-polar Apezion L 300 Amides Fatty acid methyl esters High boiling aliphatic HC Terpenoids Polydimethyl siloxane Slightly SE-30 300-350 Alkaloids* Amino acid derivatives ** Drugs# pesticides## Phenols & steroids 50% methyl50%phenyl polysiloxane Moderate OV-17 375 *, #, ##, Polyaromatic hydrocarbons Polychlorinated biphenyls 50%TFP50%MPSO Moderate OV-210 275 *,**, #, halogenated compounds, ketones, phenols 50% CYP-50% phe-me-PSO Polar OV-225 275 Nitriles, pesticides, steroids PEG Polar Carbowax 20M 225 Aldehydes, esters, ethers, phenols
    11. 11. Introduction of samples 1. All constituents must be volatile 2. Appropriate concentration 3. Must not degrade the separation Volatile analyte from Non volatile matrix: 1. 2. 3. 4. Liquid-liquid extraction Solid phase extraction  SPME Headspace sampling Cryogenic focusing
    12. 12. Injecting the sample • Split injection • Splitless injection • On-column injection Schematic diagram of an injector for packed column GC
    13. 13. Detectors in GC Thermal Conductivity
    14. 14. Another detectors • • • • Flame photometric detector Thermionic detector FT-IR (GC-FT-IR) MS (GC-MS)
    15. 15. Quantitative applications • • • • Environmental analysis Clinical analysis/forensic may include Consumer goods Petroleum industry

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