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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