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GC. Schematic of a GC Typical GC Carrier gas/ Regulator Varian 3350 Gas Chromatograph Computer Controls for Method and Output.

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Presentation on theme: "GC. Schematic of a GC Typical GC Carrier gas/ Regulator Varian 3350 Gas Chromatograph Computer Controls for Method and Output."— Presentation transcript:

1 GC

2 Schematic of a GC

3 Typical GC Carrier gas/ Regulator Varian 3350 Gas Chromatograph Computer Controls for Method and Output

4 Separation T=0 T=10’ T=20’ Injector Detector Most Interaction with Stationary Phase Least Flow of Mobile Phase

5 GC – Peak Broadening

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7 Carrier gas velocity in the column

8 Chromatography – Dead Volume Mixing

9 GC - Column

10 Columns

11 GC – Capillary Column

12

13 Separation

14 GC Liquid Phases

15 GC – Column Efficiency Packed Capillary

16 GC – Sample Capacity Effect 0.25 mm 0.53 mm

17 GC – Column Flows

18 GC – Column Performance

19 GC – Film Thickness Effect 0.25  m 1.0  m 3.0  m 5.0  m

20 GC – Isothermal and Programming C50 0 C 50 0 C 3min To C at 10 0 C/min

21 Mobile Phase

22 GC – Gases Properties

23 GC – van Deemter Plots/Curves N2N2 He H2H2

24 GC - Injectors

25 GC Capillary Injection Modes

26 GC – Injector Inserts

27 GC – Injector Linear & Repeatability of Peak Area

28 GC - Injectors SPLIT INJECTOR Advantage - Limitations Injected zone narrow Small sample aliquot avoids overloading Mass discrimination of sample components (different range of volatility) Systematic errors for quantitative analysis In trace analysis: only part of analytes to detector

29 GC- Injectors SPLITLESS INJECTOR Advantage - Limitations Avoids large tailing of solvent peak Allows transfer of main part of sample components into detector Trace analysis: favourable technique for insertion of diluted samples Recondensation of solvent at top of capillary: possible damaging stationary phase Only columns with chemically bonded phases Necessary wettability of stationary phase for condensed solvent (droplets)

30 Injection Technique and Peak Discrimination Filled Needle Hot Needle Cold On-Column

31 GC – Injector Solvent Vapours Volume

32 GC – On-Column Injector

33 GC - Injectors Advantage of on-column injector: avoids mass discrimination effects trace analysis: enables quantitative insertion of sample into column (and detector) labile components not stressed thermally

34 GC - Detectors

35 GC - FID

36 GC – Flame Ionization Detector (FID)

37 GC – FID Response to Gases Flows

38 GC – Alkali Ionization Detector (N,P)

39 GC – FID & AFID Response

40 GC – Electron Capture Detector (ECD)

41 GC - Thermal Conductivity Detector

42 GC – Atomic Emission Detector

43 GC – Detectors Performance

44 GC – IR – Detector Gas Cell

45 Peak Area Integration Qualitative and Quantitative

46 Chromatography – Sampling Rate and Accuracy 2 Hz 25 Hz

47 Chromatography – Integration Problems

48 GC – Integration Problems - Deconvolution

49 Kovatc’s Index

50 GC – Retention Indexes

51 GC – Derivatization Reagents

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55 Marine SourceAnimal Source Fatty Acids

56 Conditions Column: SP-2560, 100m x 0.25mm ID, 0.20µm film Cat. No.: Oven: 140°C (5 min) to 240°C at 4°C/min, hold 15 min Carrier: helium, 20cm/sec, 175°C Det.: FID, 260°C Inj.: 1µL Supelco 37 Component FAME Mix (10mg/mL total), split (100:1), 250°C List of components on the next slide

57 Components for SP 2560 Chromatogram Analyte Data Component (acid methyl ester) Weight (%) 1. C4:0 (Butryic) 4 2. C6:0 (Caproic) 4 3. C8:0 (Caprylic) 4 4. C10:0 (Capric) 4 5. C11:0 (Undecanoic) 2 6. C12:0 (Lauric) 4 7. C13:0 (Tridecanoic) 2 8. C14:0 (Myristic) 4 9. C14:1 (Myristoleic) C15:0 (Pentadecanoic) C15:1 (cis-10-Pentadecenoic) C16:0 (Palmitic) C16:1 (Palmitoleic) C17:0 (Heptadecanoic) C17:1 (cis-10-Heptadecenoic) C18:0 (Stearic) C18:1n9c (Oleic) C18:1n9t (Elaidic) C18:2n6c (Linoleic) C18:2n6t (Linolelaidic) C18:3n6 (g-Linolenic) C18:3n3 (a-Linolenic) C20:0 (Arachidic) C20:1n9 (cis-11-Eicosenoic) C20:2 (cis-11,14-Eicosadienoic) C20:3n6 (cis-8,11,14-Eicosatrienoic) C20:3n3 (cis-11,14,17-Eicosatrienoic) C20:4n6 (Arachidonic) C20:5n3 (cis-5,8,11,14,17-Eicosapentaenoic) C21:0 (Henicosanoic) C22:0 (Behenic) C22:1n9 (Erucic) C22:2 (cis-13,16-Docosadienoic) C22:6n3 (cis-4,7,10,13,16,19-Docosahexaenoic) C23:0 (Tricosanoic) C24:0 (Lignoceric) C24:1n9 (Nervonic) 2

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