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Multi-Dimensional Gas Chromatography State-of-the-Art. J.-M. D. Dimandja January 16, 2007. Chromatography in Context. GCxGC Instrumentation. Detector. Injector. Data Processor. Secondary Column. Primary Column. Modulator. What is Modulation?. Demodulator. Modulator. Transmission. - PowerPoint PPT Presentation
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Multi-Dimensional Gas Chromatography Multi-Dimensional Gas Chromatography State-of-the-ArtState-of-the-Art
J.-M. D. DimandjaJ.-M. D. DimandjaJanuary 16, 2007January 16, 2007
Chromatography in ContextChromatography in Context
SelectiveSelective ComprehensiveComprehensive
1D GC1D GC Sample Sample Preparation Preparation CartridgesCartridges
Conventional Conventional 1D GC1D GC
2D GC2D GC Heartcut Heartcut GC-GCGC-GC
GCxGCGCxGC
GCxGC InstrumentationGCxGC Instrumentation
Data Processor
Detector
Modulator
Injector
PrimaryColumn
SecondaryColumn
What is Modulation?What is Modulation?
AudioSignal
AMFM
Modulator Demodulator
Transmission DesiredAudio Signal
1st DimensionGC Signal
Modulator Demodulator
TransmissionThrough 2nd
GC Dimension
DesiredMulti-dimensional
Signal
Role of the GCxGC ModulatorRole of the GCxGC Modulator
Amplitude ModulationAmplitude ModulationFrequency ModulationFrequency ModulationPhase ModulationPhase Modulation
The modulator plays a key role in the The modulator plays a key role in the optimization of a GCxGC methodoptimization of a GCxGC method
Types of GCxGC ModulatorsTypes of GCxGC ModulatorsThermal ModulatorsThermal ModulatorsValve ModulatorsValve Modulators
Will be covered by Prof. SeeleyWill be covered by Prof. Seeley
Modulator Figures-of-MeritModulator Figures-of-MeritSampling efficiencySampling efficiencyTemperature operating rangeTemperature operating rangeTechnical sophisticationTechnical sophisticationRuggednessRuggednessCostCost
Evolution of Thermal ModulatorsEvolution of Thermal Modulators
ResistorsResistorsThermal scannersThermal scannersThermal jets Thermal jets
Thermal Resistor PrincipleThermal Resistor PrincipleResistive heatingResistive heatingRapid cooling due to low thermal mass of Rapid cooling due to low thermal mass of
the resistive film the resistive film
Rearview DefoggerRearview Defogger
Defogger OperationDefogger Operation
Resistive paint Resistive paint heatedheated
Defogging occursDefogging occurs
Napa Defogger kitNapa Defogger kit
The Original Resistor The Original Resistor (Liu/Phillips, 1988)(Liu/Phillips, 1988)
Stationary Phase
Electrically Conductive Paint
Resistor Pros/ConsResistor Pros/ConsPoorPoor GoodGood ExcellentExcellent
Sampling EfficiencySampling Efficiency XX
Temperature RangeTemperature Range XX
Technical Technical SophisticationSophistication
XX
RuggednessRuggedness XX
CostCost XX
ImprovementsImprovementsTwo-stage modulation (Liu, 1989)Two-stage modulation (Liu, 1989)Thicker stationary phase (Liu, 1990)Thicker stationary phase (Liu, 1990)Dry-ice resistor (Venkatramani, 1991)Dry-ice resistor (Venkatramani, 1991)Stainless-steel, multi-stage resistor Stainless-steel, multi-stage resistor
(Burger, 2003)(Burger, 2003)
Resistor SummaryResistor Summary Interfaced with HRMS (1994) and TOF MS Interfaced with HRMS (1994) and TOF MS
(1996)(1996)Academia (prototype development), Academia (prototype development),
Industry (Shell), government R&D (CDC)Industry (Shell), government R&D (CDC)Cheap and easy to assemble, but not Cheap and easy to assemble, but not
commercially viablecommercially viable
Thermal Scanning PrincipleThermal Scanning Principle
Mechanically activated modulator that scans a given section of the columnto produce the modulation.
1
2
Dual-Oven Heat Shuttle (Xu, 1993)Dual-Oven Heat Shuttle (Xu, 1993)
12
Single-Oven Heat Shuttle Single-Oven Heat Shuttle (Xu, 1994)(Xu, 1994)
12
Inside-Oven Cryo-Shuttle Inside-Oven Cryo-Shuttle (Marriott, 1995)(Marriott, 1995)
12
Inside-Oven Heat Shuttle -- Inside-Oven Heat Shuttle -- Thermal Sweeper Thermal Sweeper
(Ledford/Phillips, 1997)(Ledford/Phillips, 1997)
12
Thermal Scanner Pros/ConsThermal Scanner Pros/ConsPoorPoor GoodGood ExcellentExcellent
Sampling EfficiencySampling Efficiency XX
Temperature RangeTemperature Range XX
Technical Technical SophisticationSophistication
XX
RuggednessRuggedness XX
CostCost XX
Thermal Scanner SummaryThermal Scanner SummaryFirst “commercial” system (Sweeper, First “commercial” system (Sweeper,
1997)1997)Petroleum industry, government R&D Petroleum industry, government R&D
(CDC, CGA)(CDC, CGA)Data processing issues (no software for Data processing issues (no software for
automated visualization and/or automated visualization and/or quantitation)quantitation)
Jet Modulator PrincipleJet Modulator PrincipleActive cooling and heating stagesActive cooling and heating stagesThermal scanners only have one active Thermal scanners only have one active
stage (either heating or cooling, but not stage (either heating or cooling, but not both)both)
Single-Stage, Dual-Jet Single-Stage, Dual-Jet (Beens, 2001)(Beens, 2001)
Trapping phase
Single-Stage, Dual-JetSingle-Stage, Dual-Jet
Release phase
Two-Stage, Quad-Jet Modulation Two-Stage, Quad-Jet Modulation (Ledford, 2001)(Ledford, 2001)
TRAP
Two-Stage, Quad-Jet ModulationTwo-Stage, Quad-Jet Modulation
FOCUS
Two-Stage, Quad-Jet ModulationTwo-Stage, Quad-Jet Modulation
RELEASE
Two-Stage, Dual-Jet Modulation Two-Stage, Dual-Jet Modulation (Ledford, 2002)(Ledford, 2002)
Two-Stage, Dual-Jet ModulationTwo-Stage, Dual-Jet Modulation
Two-Stage, Dual-Jet ModulationTwo-Stage, Dual-Jet Modulation
Two-Stage, Dual-Jet ModulationTwo-Stage, Dual-Jet Modulation
Thermal Jets Pros/ConsThermal Jets Pros/ConsPoorPoor GoodGood ExcellentExcellent
Sampling EfficiencySampling Efficiency XX
Temperature RangeTemperature Range XX
Technical Technical SophisticationSophistication
XX
RuggednessRuggedness XX
CostCost XX
Thermal Jet SummaryThermal Jet SummaryCurent commercially available state-of-Curent commercially available state-of-
the-art in GCxGCthe-art in GCxGC Industry, academia, governmentIndustry, academia, governmentAchilles heel: consumablesAchilles heel: consumables
Gaines/Frysinger solutionGaines/Frysinger solutionHarynuk/Gorecki solutionHarynuk/Gorecki solution
ConclusionsConclusions
InstrumentInstrumentDevelopmentDevelopment
ModulationModulation
ApplicationApplicationDevelopmentDevelopment
DemodulationDemodulation(Data Processing (Data Processing Software)Software)