gc. schematic of a gc typical gc carrier gas/ regulator varian 3350 gas chromatograph computer...
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GCGC
Schematic of a GCSchematic of a GC
Typical GCTypical GC
Carrier gas/Carrier gas/RegulatorRegulator
Varian 3350 Gas Varian 3350 Gas ChromatographChromatograph
Computer Controls forComputer Controls forMethod and Output Method and Output
SeparationSeparation
T=0
T=10’
T=20’
InjectorInjector DetectorDetector
MostMost Interaction with Stationary PhaseInteraction with Stationary Phase LeastLeast
Flow of Mobile PhaseFlow of Mobile Phase
GC – Peak BroadeningGC – Peak Broadening
Carrier gas velocity in the column
Chromatography – Dead Volume MixingChromatography – Dead Volume Mixing
GC - ColumnGC - Column
ColumnsColumns
GC – Capillary ColumnGC – Capillary Column
SeparationSeparation
GC Liquid Phases
GC – Column EfficiencyGC – Column Efficiency
Packed Capillary
GC – Sample Capacity EffectGC – Sample Capacity Effect
0.25 mm 0.53 mm
GC – Column FlowsGC – Column Flows
GC – Column PerformanceGC – Column Performance
GC – Film Thickness EffectGC – Film Thickness Effect
0.25m
1.0m
3.0m
5.0m
GC – Isothermal and ProgrammingGC – Isothermal and Programming
1050C 500C
500C 3minTo 1400C at100C/min
Mobile PhaseMobile Phase
GC – Gases PropertiesGC – Gases Properties
GC – van Deemter Plots/CurvesGC – van Deemter Plots/Curves
N2
He
H2
GC - InjectorsGC - Injectors
GCGCCapillaryCapillaryInjection Injection
ModesModes
GC – Injector InsertsGC – Injector Inserts
GC – Injector Linear & Repeatability of Peak AreaGC – Injector Linear & Repeatability of Peak Area
GC - InjectorsGC - Injectors
SPLIT INJECTORAdvantage - 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
GC- InjectorsGC- 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)
Injection Technique and Peak DiscriminationInjection Technique and Peak Discrimination
Filled Needle
Hot Needle
Cold On-Column
GC – Injector Solvent Vapours Volume GC – Injector Solvent Vapours Volume
GC – On-Column InjectorGC – On-Column Injector
GC - InjectorsGC - 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
GC - DetectorsGC - Detectors
GC - FID
GC – Flame Ionization Detector (FID)GC – Flame Ionization Detector (FID)
GC – FID Response to Gases FlowsGC – FID Response to Gases Flows
GC – Alkali Ionization Detector (N,P)GC – Alkali Ionization Detector (N,P)
GC – FID & AFID ResponseGC – FID & AFID Response
GC – Electron Capture Detector (ECD)GC – Electron Capture Detector (ECD)
GC - Thermal Conductivity Detector
GC – Atomic Emission DetectorGC – Atomic Emission Detector
GC – Detectors PerformanceGC – Detectors Performance
GC – IR – Detector Gas CellGC – IR – Detector Gas Cell
Peak Area IntegrationPeak Area IntegrationQualitative and QuantitativeQualitative and Quantitative
Chromatography – Sampling Rate and AccuracyChromatography – Sampling Rate and Accuracy
2 Hz
25 Hz
Chromatography – Integration ProblemsChromatography – Integration Problems
GC – Integration Problems - DeconvolutionGC – Integration Problems - Deconvolution
Kovatc’s IndexKovatc’s Index
GC – Retention IndexesGC – Retention Indexes
GC – Derivatization ReagentsGC – Derivatization Reagents
Marine Source Animal Source
Fatty Acids
Conditions Column: SP-2560, 100m x 0.25mm ID, 0.20µm filmCat. No.: 24056Oven: 140°C (5 min) to 240°C at 4°C/min, hold 15 minCarrier: helium, 20cm/sec, 175°CDet.: FID, 260°CInj.: 1µL Supelco 37 Component FAME Mix (10mg/mL total), split (100:1), 250°C
List of components on the next slide
Components for SP 2560 ChromatogramComponents for SP 2560 ChromatogramAnalyte DataAnalyte Data Component (acid methyl Component (acid methyl
ester) Weight (%)ester) Weight (%)1. C4:0 (Butryic) 41. C4:0 (Butryic) 42. C6:0 (Caproic) 42. C6:0 (Caproic) 43. C8:0 (Caprylic) 43. C8:0 (Caprylic) 44. C10:0 (Capric) 44. C10:0 (Capric) 45. C11:0 (Undecanoic) 25. C11:0 (Undecanoic) 26. C12:0 (Lauric) 46. C12:0 (Lauric) 47. C13:0 (Tridecanoic) 27. C13:0 (Tridecanoic) 28. C14:0 (Myristic) 48. C14:0 (Myristic) 49. C14:1 (Myristoleic) 29. C14:1 (Myristoleic) 210. C15:0 (Pentadecanoic) 210. C15:0 (Pentadecanoic) 211. C15:1 11. C15:1 (cis(cis-10-Pentadecenoic) 2-10-Pentadecenoic) 212. C16:0 (Palmitic) 612. C16:0 (Palmitic) 613. C16:1 (Palmitoleic) 213. C16:1 (Palmitoleic) 214. C17:0 (Heptadecanoic) 214. C17:0 (Heptadecanoic) 215. C17:1 15. C17:1 (cis(cis-10-Heptadecenoic) 2-10-Heptadecenoic) 216. C18:0 (Stearic) 416. C18:0 (Stearic) 417. C18:1n9c (Oleic) 417. C18:1n9c (Oleic) 418. C18:1n9t (Elaidic) 218. C18:1n9t (Elaidic) 219. C18:2n6c (Linoleic)19. C18:2n6c (Linoleic) 2 2
20. C18:2n6t (Linolelaidic) 220. C18:2n6t (Linolelaidic) 221. C18:3n6 (g-Linolenic) 221. C18:3n6 (g-Linolenic) 222. C18:3n3 (a-Linolenic) 222. C18:3n3 (a-Linolenic) 223. C20:0 (Arachidic) 423. C20:0 (Arachidic) 424. C20:1n9 24. C20:1n9 (cis(cis-11-Eicosenoic) 2-11-Eicosenoic) 225. C20:2 25. C20:2 (cis(cis-11,14-Eicosadienoic) 2-11,14-Eicosadienoic) 226. C20:3n6 26. C20:3n6 (cis(cis-8,11,14-Eicosatrienoic) 2-8,11,14-Eicosatrienoic) 227. C20:3n3 27. C20:3n3 (cis(cis-11,14,17-Eicosatrienoic) 2-11,14,17-Eicosatrienoic) 228. C20:4n6 (Arachidonic) 228. C20:4n6 (Arachidonic) 229. C20:5n3 29. C20:5n3 (cis(cis-5,8,11,14,17-Eicosapentaenoic) 2-5,8,11,14,17-Eicosapentaenoic) 230. C21:0 (Henicosanoic) 230. C21:0 (Henicosanoic) 231. C22:0 (Behenic) 431. C22:0 (Behenic) 432. C22:1n9 (Erucic) 232. C22:1n9 (Erucic) 233. C22:233. C22:2 (cis (cis-13,16-Docosadienoic) 2-13,16-Docosadienoic) 234. C22:6n334. C22:6n3 (cis(cis-4,7,10,13,16,19-Docosahexaenoic) 2-4,7,10,13,16,19-Docosahexaenoic) 235. C23:0 (Tricosanoic) 235. C23:0 (Tricosanoic) 236. C24:0 (Lignoceric) 436. C24:0 (Lignoceric) 437. C24:1n9 (Nervonic) 237. C24:1n9 (Nervonic) 2
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