tfh 2005 ws. lcgc adsorption/verteilungpacked/verteilung normal phase [pol-unp] reversed phase...
TRANSCRIPT
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LC GCAdsorption/Verteilung Packed/Verteilung
Normal Phase [pol-unp]
Reversed Phase [unp-pol]
Kapillare Glas / FSOF Modifizierung/HTS
Irregular / Regular shapeParticle size, Pores
Polysiloxanphasen / crosslinked / chiral
Desaktivierung / pH Stabilität Capillary Adsorption
Reduced Particle size FAST GC / 2D GC
Worldwide Repeatability Retention Time Locking
SPME
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Factors Affecting Resolution
k`= K / ß
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Modulators
Thermal modulator
Cryogenic modulator
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Oberflächenchemie
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Cross section of a Fused Silica Column Open Tubular
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PHASEN
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Choosing the Bonded Phase
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Choosing the Bonded Phase
R = C14 alkyl
R1 = isopropyl shielding
Diisopropyl side groups provide steric protection against low pH
Triple endcapping, shielding
PG = polar amide group
Polar amide group embedded in a long alkyl chain reduces interactiions between basic analytes and silica support
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PACKUNG HPLC
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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.
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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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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.
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Kieselgelträgermaterial
Xerogel(Sil Typ)
Rx-SIL(Sol Typ)Zorbax
STRUKTUR: GLEICHMÄSSIGE PARTKEL“SCHWAMM-STRUKTUR,” POLYMERES NETZWERK
POROSITÄT (%):
PARTIKEL GRÖSSE/OBERFLÄCHE (M2/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
Scale: = 1 µm
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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.
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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.
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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
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Bonding Type
Si
R
R
(CH2)17CH3Si
CH3
CH3
(CH2)17CH3XOH +monomeric
bonding
Si
CH3
X
(CH2)17CH3X+polymeric
bonding
OH
OH O
O
Si
CH3
(CH2)17CH3
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.
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Acidity
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Mechanisms
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Thomas Mann
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SPME
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MULTIKAPILLARE
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FFF
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FF
F
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Pyrolyse
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Terrorismmethods: quick, facile
Pyrolyse - (GC) - MS
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Pharmahilfsstoffe:Pharmahilfsstoffe:
Synthetische Polymere,Synthetische Polymere,Biopolymere,Biopolymere,andere biogene hochmole-andere biogene hochmole-kulare Substanzenkulare Substanzen
nicht oder nicht ausreichend flüchtig
GC-AnalytikGC-Analytik
Pyrolyse als Bindeglied:Pyrolyse als Bindeglied:Thermischer Abbau des hochmolekularenThermischer Abbau des hochmolekularen
Probenmaterials in niedermolekulare, Probenmaterials in niedermolekulare, flüchtigeflüchtige Pyrolyseprodukte Pyrolyseprodukte
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Charakterisierung SAG Hilfsstoffe