gc. schematic of a gc typical gc carrier gas/ regulator varian 3350 gas chromatograph computer...
TRANSCRIPT
![Page 1: GC. Schematic of a GC Typical GC Carrier gas/ Regulator Varian 3350 Gas Chromatograph Computer Controls for Method and Output](https://reader035.vdocuments.us/reader035/viewer/2022081417/551b3b05550346cf5a8b6636/html5/thumbnails/1.jpg)
GCGC
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Schematic of a GCSchematic of a GC
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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
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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
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GC – Peak BroadeningGC – Peak Broadening
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Carrier gas velocity in the column
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Chromatography – Dead Volume MixingChromatography – Dead Volume Mixing
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GC - ColumnGC - Column
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ColumnsColumns
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GC – Capillary ColumnGC – Capillary Column
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SeparationSeparation
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GC Liquid Phases
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GC – Column EfficiencyGC – Column Efficiency
Packed Capillary
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GC – Sample Capacity EffectGC – Sample Capacity Effect
0.25 mm 0.53 mm
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GC – Column FlowsGC – Column Flows
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GC – Column PerformanceGC – Column Performance
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GC – Film Thickness EffectGC – Film Thickness Effect
0.25m
1.0m
3.0m
5.0m
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GC – Isothermal and ProgrammingGC – Isothermal and Programming
1050C 500C
500C 3minTo 1400C at100C/min
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Mobile PhaseMobile Phase
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GC – Gases PropertiesGC – Gases Properties
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GC – van Deemter Plots/CurvesGC – van Deemter Plots/Curves
N2
He
H2
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GC - InjectorsGC - Injectors
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GCGCCapillaryCapillaryInjection Injection
ModesModes
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GC – Injector InsertsGC – Injector Inserts
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GC – Injector Linear & Repeatability of Peak AreaGC – Injector Linear & Repeatability of Peak Area
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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
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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)
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Injection Technique and Peak DiscriminationInjection Technique and Peak Discrimination
Filled Needle
Hot Needle
Cold On-Column
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GC – Injector Solvent Vapours Volume GC – Injector Solvent Vapours Volume
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GC – On-Column InjectorGC – On-Column Injector
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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
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GC - DetectorsGC - Detectors
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GC - FID
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GC – Flame Ionization Detector (FID)GC – Flame Ionization Detector (FID)
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GC – FID Response to Gases FlowsGC – FID Response to Gases Flows
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GC – Alkali Ionization Detector (N,P)GC – Alkali Ionization Detector (N,P)
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GC – FID & AFID ResponseGC – FID & AFID Response
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GC – Electron Capture Detector (ECD)GC – Electron Capture Detector (ECD)
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GC - Thermal Conductivity Detector
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GC – Atomic Emission DetectorGC – Atomic Emission Detector
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GC – Detectors PerformanceGC – Detectors Performance
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GC – IR – Detector Gas CellGC – IR – Detector Gas Cell
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Peak Area IntegrationPeak Area IntegrationQualitative and QuantitativeQualitative and Quantitative
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Chromatography – Sampling Rate and AccuracyChromatography – Sampling Rate and Accuracy
2 Hz
25 Hz
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Chromatography – Integration ProblemsChromatography – Integration Problems
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GC – Integration Problems - DeconvolutionGC – Integration Problems - Deconvolution
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Kovatc’s IndexKovatc’s Index
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GC – Retention IndexesGC – Retention Indexes
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GC – Derivatization ReagentsGC – Derivatization Reagents
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Marine Source Animal Source
Fatty Acids
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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
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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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