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GAS CHROMATOGRAPH. GAS CHROMATOGRAPH Principle: Which type of compounds can analyse? Volatile Thermostable.

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Presentation on theme: "GAS CHROMATOGRAPH. GAS CHROMATOGRAPH Principle: Which type of compounds can analyse? Volatile Thermostable."— Presentation transcript:

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2 GAS CHROMATOGRAPH

3 Principle: Which type of compounds can analyse? Volatile Thermostable

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5 Carrier gas supply: Hydrogen, Helium, Nitrogen, Argon
Requirements of a carrier gas: Inert High purity Easy available Cheap Less risk of explosion Best column performance Compatible with the stationary phase and the sample and detector used

6 Carrier gas flow regulator
Carrier gas cylinder Carrier gas flow regulator Carrier gas cylinder, Carrier gas flow regulator

7 Sample injection devices:
Manual - Direct Injection Automated - Auto sampler - Purge and Trap Commercial GC- Split & Splitless inj.& On column inj. Liquids Gases Solids

8 Gases Position -I Position -II Position -I

9 .>0.1%,0.01% SPLIT RATIO:1/49,25/49UL

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11 On-Column Injector

12 Columns: Column selection Column length Column diameter
Column efficiency Column head pressure Column cost Column diameter

13 GC Columns Packed columns Capillary columns/Open tubular
Typically a glass or stainless steel coil. 1-5 total length and inner diameter:2 & 4mm Packing particles diameter: 100 to 250 micrometers porous-layer open tubular (PLOT) column support-coated open tubular(SCOT) column wall coated open tubular column (WCOT)

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16 Packed Capillary

17 List of common stationary phases and their polarities
Column Stationary Phase Polarity Diatomaceous Earth (SiO2, Al2O3, Fe2O3, CaO, MgO, Na2O, and K2O) relatively non-polar Clay Celite Squalane (C30H62) (purified with charcoal and alumina) non-polar Hexadecane Apolane-87 (C87H176) Apiexon Greases (purified with charcoal and alumina) Dialkyl Phthalates moderately polar Tetrachlorophthalates Polyethylene Glycol (Carbowax 20M) Polysiloxanes non-polar-polar (depending on the R group attached)

18 List of functional groups attached to the stationary phase and their polarities
Stationary Phase Functional Group Polarity Polyester Phases Highly Polar -OH Polar -CN -CO Hydrocarbons Non-polar Dialkyl Siloxanes

19 Analyte Functional Groups (Polar to Non-polar)
Water Acids Alcohols Amines Amides Aldehydes Ketones Esters Ethers Aromatics Hydrocarbons

20 Column Oven The oven can be operated in two manners:
A gas chromatography oven, open to show a capillary column The oven can be operated in two manners:  isothermal programming temperature programming

21 The effect of column temperature on the shape of the peaks

22 Detection Systems Characteristics of the Ideal Detector: The ideal detector for gas chromatography has the following characteristics: 1. Adequate sensitivity 2. Good stability and reproducibility. 3. A linear response to solutes that extends over several orders of magnitude. 4. A temperature range from room temperature to at least 400oC.

23 Characteristics of the Ideal Detector
5. A short response time that is independent of flow rate. 6. High reliability and ease of use. 7. Similarity in response toward all solutes or a highly selective response toward one or more classes of solutes. 8. Nondestructive of sample.

24 Type of Detector Applicable Samples Detection Systems
Flame Ionization (FID)  Hydrocarbons  Thermal Conductivity (TCD)  Universal  Electron-Capture (ECD)  Halogenated hydrocarbons  Argon ionisation detector Organic compounds Nitrogen Phosphorous detector Molecules containing N2/P

25 These properties allow FID high sensitivity and low noise.
Flame Ionization Detectors Advantageous : the detector is unaffected by flow rate, noncombustible gases and water.  These properties allow FID high sensitivity and low noise.  relatively easy to use.  Disadvantages: this technique does require flammable gas and also destroys the sample. 

26 The Electron Capture Detector
used for detecting environmental samples as the device selectively detects organic compounds with moieties such as halogens, peroxides, quinones and nitro groups . best suited in applications where traces quantities of chemicals such as pesticides are to be detected high selectivity and sensitivity towards certain organic species with electronegative functional groups. 

27 Thermal conductivity detector
advantages : ease and simplicity of use application to inorganic and organic compounds, and the ability of the analyte to be collected after separation and detection.  drawback : TCD is the low sensitivity of the instrument in relation to other detection methods, in addition to flow rate and concentration dependency

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29 Nitrogen Phosphorus Detector

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