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TFH 2005 WS. LCGC Adsorption/VerteilungPacked/Verteilung Normal Phase [pol-unp] Reversed Phase [unp-pol] Kapillare Glas / FS OF Modifizierung/HTS Irregular.

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Presentation on theme: "TFH 2005 WS. LCGC Adsorption/VerteilungPacked/Verteilung Normal Phase [pol-unp] Reversed Phase [unp-pol] Kapillare Glas / FS OF Modifizierung/HTS Irregular."— Presentation transcript:

1 TFH 2005 WS

2 LCGC Adsorption/VerteilungPacked/Verteilung Normal Phase [pol-unp] Reversed Phase [unp-pol] Kapillare Glas / FS OF Modifizierung/HTS Irregular / Regular shape Particle size, Pores Polysiloxanphasen / crosslinked / chiral Desaktivierung / pH Stabilität Capillary Adsorption Reduced Particle size FAST GC / 2D GC Worldwide Repeatability Retention Time Locking SPME

3 TFH 2005 WS Factors Affecting Resolution k`= K / ß

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6 Modulators Thermal modulator Cryogenic modulator

7 TFH 2005 WS Oberflächenchemie

8 TFH 2005 WS Cross section of a Fused Silica Column Open Tubular

9 TFH 2005 WS PHASEN

10 TFH 2005 WS Choosing the Bonded Phase

11 TFH 2005 WS Choosing the Bonded Phase R = C 14 alkyl R1 = isopropyl shielding Diisopropyl side groups provide steric protection against low p H Triple endcapping, shielding PG = polar amide group Polar amide group embedded in a long alkyl chain reduces interactiions between basic analytes and silica support

12 TFH 2005 WS PACKUNG HPLC

13 TFH 2005 WS Particle Shape Effect on chromatography Spherical particles offer reduced back pressures and longer column life when using viscous mobile phases like 50:50 MeOH:H2O.

14 TFH 2005 WS Particle Size Effect on chromatography Smaller particles offer higher efficiency, but also cause higher backpressure. Choose 3 µm particles for resolving complex, multi-component samples. Otherwise, choose 5 or 10µm packings.

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23 Surface Area Effect on chromatography High surface area generally provides greater retention, capacity and resolution for separating complex, multi-component samples. Low surface area packings generally equilibrate quickly, especially important in gradient analyses.

24 TFH 2005 WS Kieselgelträgermaterial Xerogel (Sil Typ) Rx-SIL (Sol Typ) Zorbax STRUKTUR:GLEICHMÄSSIGE PARTKELSCHWAMM-STRUKTUR, POLYMERES NETZWERK POROSITÄT (%): PARTIKEL GRÖSSE/ OBERFLÄCHE (M 2 /G) MECHAN. STABILITÄT: HOHE pH-STABILITÄT: REINHEIT: PORENGRÖSSE, PARTIKELGRÖSSE VERTEILUNG 50 80A/180 HOCH GUT HOCH ENG 70 100A/300 MITTEL SCHLECHT NIEDER - HOCH BREIT

25 TFH 2005 WS Pore Size Effect on chromatography Larger pores allow larger solute molecules to be retained longer through maximum exposure to the surface area of the particles. Choose a pore size of 150Å or less for sample MW 2000. Choose a pore size of 300Å or greater for sample MW > 2000.

26 TFH 2005 WS Endcapping Effect on chromatography Endcapping reduces peak-tailing of polar solutes that interact excessively with the otherwise exposed, mostly acidic silanols. Non-endcapped packings provide a different selectivity than do endcapped packings, especially for such polar samples.

27 TFH 2005 WS Carbon Load Effect on chromatography Higher carbon loads generally offer greater resolution and longer run times. Low carbon loads shorten run times and many show a different selectivity

28 TFH 2005 WS Bonding Type Monomeric bonding offers increased mass transfer rates, higher column efficiency, and faster column equilibration. Polymeric bonding offers increased column stability, particularly when highly aqueous mobile phases are used. Polymeric bonding also enables the column to accept higher sample loading.

29 TFH 2005 WS Acidity

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32 Mechanisms

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35 Thomas Mann

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37 SPME

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48 MULTIKAPILLARE

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50 FFF

51 TFH 2005 WS FFF

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53 Pyrolyse

54 TFH 2005 WS Terrorism methods: quick, facile Pyrolyse - (GC) - MS

55 TFH 2005 WS Pharmahilfsstoffe: Synthetische Polymere, Biopolymere, andere biogene hochmole- kulare Substanzen nicht oder nicht ausreichend flüchtig GC-Analytik Pyrolyse als Bindeglied: Thermischer Abbau des hochmolekularen Probenmaterials in niedermolekulare, flüchtige Pyrolyseprodukte

56 TFH 2005 WS Charakterisierung SAG Hilfsstoffe


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