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Multi-Dimensional Gas Chromatography State-of-the-Art J. -M. D. Dimandja January 16, 2007 Multi-Dimensional Gas Chromatography State-of-the-Art J. -M. D. Dimandja January 16, 2007

Chromatography in Context Selective 1 D GC 2 D GC Comprehe nsive Sample Convention Chromatography in Context Selective 1 D GC 2 D GC Comprehe nsive Sample Convention Preparation al 1 D GC Cartridges Heartcut GC-GC GCx. GC

GCx. GC Instrumentation Detector Injector Data Processor Primary Column Modulator Secondary Column GCx. GC Instrumentation Detector Injector Data Processor Primary Column Modulator Secondary Column

What is Modulation? Demodulator Modulator Audio Signal AM FM Transmission Demodulator Modulator 1 st What is Modulation? Demodulator Modulator Audio Signal AM FM Transmission Demodulator Modulator 1 st Dimension GC Signal Desired Audio Signal Transmission Through 2 nd GC Dimension Desired Multi-dimensional Signal

Role of the GCx. GC Modulator Amplitude Modulation l Frequency Modulation l Phase Modulation Role of the GCx. GC Modulator Amplitude Modulation l Frequency Modulation l Phase Modulation l l The modulator plays a key role in the optimization of a GCx. GC method

Types of GCx. GC Modulators Thermal Modulators l Valve Modulators l l Will be Types of GCx. GC Modulators Thermal Modulators l Valve Modulators l l Will be covered by Prof. Seeley

Modulator Figures-of-Merit Sampling efficiency l Temperature operating range l Technical sophistication l Ruggedness l Modulator Figures-of-Merit Sampling efficiency l Temperature operating range l Technical sophistication l Ruggedness l Cost l

Evolution of Thermal Modulators Resistors l Thermal scanners l Thermal jets l Evolution of Thermal Modulators Resistors l Thermal scanners l Thermal jets l

Thermal Resistor Principle Resistive heating l Rapid cooling due to low thermal mass of Thermal Resistor Principle Resistive heating l Rapid cooling due to low thermal mass of the resistive film l

Rearview Defogger Rearview Defogger

Defogger Operation l Resistive paint heated l Defogging occurs Defogger Operation l Resistive paint heated l Defogging occurs

Napa Defogger kit Napa Defogger kit

The Original Resistor (Liu/Phillips, 1988) Conductive Paint Electrically Stationary Phase The Original Resistor (Liu/Phillips, 1988) Conductive Paint Electrically Stationary Phase

Resistor Pros/Cons Poor Good Sampling Efficiency X Temperature Range Excellent X Technical Sophistication Ruggedness Resistor Pros/Cons Poor Good Sampling Efficiency X Temperature Range Excellent X Technical Sophistication Ruggedness Cost X X X

Improvements Two-stage modulation (Liu, 1989) l Thicker stationary phase (Liu, 1990) l Dry-ice resistor Improvements Two-stage modulation (Liu, 1989) l Thicker stationary phase (Liu, 1990) l Dry-ice resistor (Venkatramani, 1991) l Stainless-steel, multi-stage resistor (Burger, 2003) l

Resistor Summary Interfaced with HRMS (1994) and TOF MS (1996) l Academia (prototype development), Resistor Summary Interfaced with HRMS (1994) and TOF MS (1996) l Academia (prototype development), Industry (Shell), government R&D (CDC) l Cheap and easy to assemble, but not commercially viable l

Thermal Scanning Principle Mechanically activated modulator that scans a given section of the column Thermal Scanning Principle Mechanically activated modulator that scans a given section of the column to produce the modulation. 1 2

Dual-Oven Heat Shuttle (Xu, 1993) 1 2 Dual-Oven Heat Shuttle (Xu, 1993) 1 2

Single-Oven Heat Shuttle (Xu, 1994) 1 2 Single-Oven Heat Shuttle (Xu, 1994) 1 2

Inside-Oven Cryo-Shuttle (Marriott, 1995) 1 2 Inside-Oven Cryo-Shuttle (Marriott, 1995) 1 2

Inside-Oven Heat Shuttle -Thermal Sweeper (Ledford/Phillips, 1997) 1 2 Inside-Oven Heat Shuttle -Thermal Sweeper (Ledford/Phillips, 1997) 1 2

Thermal Scanner Pros/Cons Poor Good Sampling Efficiency X Temperature Range X Technical Sophistication X Thermal Scanner Pros/Cons Poor Good Sampling Efficiency X Temperature Range X Technical Sophistication X Ruggedness X Cost X Excellent

Thermal Scanner Summary First “commercial” system (Sweeper, 1997) l Petroleum industry, government R&D (CDC, Thermal Scanner Summary First “commercial” system (Sweeper, 1997) l Petroleum industry, government R&D (CDC, CGA) l Data processing issues (no software for automated visualization and/or quantitation) l

Jet Modulator Principle Active cooling and heating stages l Thermal scanners only have one Jet Modulator Principle Active cooling and heating stages l Thermal scanners only have one active stage (either heating or cooling, but not both) l

Single-Stage, Dual-Jet (Beens, 2001) Trapping phase Single-Stage, Dual-Jet (Beens, 2001) Trapping phase

Single-Stage, Dual-Jet Release phase Single-Stage, Dual-Jet Release phase

Two-Stage, Quad-Jet Modulation (Ledford, 2001) TRAP Two-Stage, Quad-Jet Modulation (Ledford, 2001) TRAP

Two-Stage, Quad-Jet Modulation FOCUS Two-Stage, Quad-Jet Modulation FOCUS

Two-Stage, Quad-Jet Modulation RELEASE Two-Stage, Quad-Jet Modulation RELEASE

Two-Stage, Dual-Jet Modulation (Ledford, 2002) Two-Stage, Dual-Jet Modulation (Ledford, 2002)

Two-Stage, Dual-Jet Modulation Two-Stage, Dual-Jet Modulation

Two-Stage, Dual-Jet Modulation Two-Stage, Dual-Jet Modulation

Two-Stage, Dual-Jet Modulation Two-Stage, Dual-Jet Modulation

Thermal Jets Pros/Cons Poor Good Excellent Sampling Efficiency X Temperature Range X Technical Sophistication Thermal Jets Pros/Cons Poor Good Excellent Sampling Efficiency X Temperature Range X Technical Sophistication X Ruggedness Cost X X

Thermal Jet Summary Curent commercially available state-of-theart in GCx. GC l Industry, academia, government Thermal Jet Summary Curent commercially available state-of-theart in GCx. GC l Industry, academia, government l Achilles heel: consumables l l Gaines/Frysinger solution l Harynuk/Gorecki solution

Conclusions Instrument Development Modulation Application Development Demodulation (Data Processing Software) Conclusions Instrument Development Modulation Application Development Demodulation (Data Processing Software)