Preparative Liquid Chromatography

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Table of contents

CHAPTER 1. CHARACTERIZATION OF OXYGENATED SPECIES IN COAL LIQUEFACTION PRODUCTS: AN OVERVIEW 
1.1 Introduction
1.2 Properties of coal-derived liquids
1.3 Characterization by One-dimensional Gas Chromatography
1.3.1 Selective characterization of oxygenates in coal-derived liquids by GC-AED
1.3.2 Applications of GC-MS to characterize oxygenates in coal liquids
1.4 Applications of Two-dimensional Gas Chromatography to unravel oxygenated structures in DCL
1.5 Characterization by Liquid Chromatography
1.5.1 Preparative Liquid Chromatography
1.5.2 High Performance Liquid Chromatography
1.6 Selective analysis of phenols and alcohols by NMR spectroscopy
1.7 Characterization of oxygenated compounds by FT-ICR/MS
1.8 Conclusion
CHAPTER 2. INVESTIGATING GC×GC TO OPTIMIZE THE SEPARATION OF OXYGENATED COMPOUNDS IN A DIRECT COAL LIQUEFACTION MIDDLE DISTILLATE
2.1 Introduction
2.2 Experimental
2.2.1 Samples
2.2.2 GC×GC-FID setup
2.2.3 GC×GC-ToF/MS
2.2.4 Data handling
2.2.5 Two-dimensional decisive factors
2.3 Results and discussion
2.3.1 Investigated configurations
2.3.2 Selection of the most adapted configuration
2.3.3 GC×GC-ToF/MS analysis of the selected configuration
2.4 Conclusion
CHAPTER 3. USING GAS CHROMATOGRAPHY TO CHARACTERIZE A DIRECT COAL LIQUEFACTION NAPHTHA
3.1 Introduction
3.2 Experimental
3.2.1 Materials
3.2.2 GC-ToF/MS setup
3.2.3 GC-GC-FID setup
3.2.4 GC×GC-FID
3.2.5 GC×GC-ToF/MS
3.3 Results and discussion
3.3.1 Speciation of oxygenated compounds by GC-ToF/MS
3.3.2 Towards a detailed characterization of oxygenates by GC-GC-FID
3.3.3 Speciation of oxygenated compounds using GC×GC
3.3.4 Comparison of the three techniques
3.4 Conclusion
CHAPTER 4. A NOVEL ANALYTICAL APPROACH FOR OXYGEN SPECIATION IN COAL-DERIVED LIQUIDS 
4.1 Introduction
4.2 Materials and methods
4.2.1 Samples
4.2.2 Gas chromatography analysis
4.2.3 Mass spectrometry analysis
4.2.4 31P Nuclear Magnetic Resonance analysis
4.2.5 UV-visible spectroscopy analysis
4.3 Results and discussion
4.3.1 Methodology
4.3.2 Detailed quantification of alcohols and phenols by GC×GC
4.3.3 Identification of phenols and carboxylic acids by FT-ICR/MS in the coal derived AGO
4.3.4 Global quantification of alcohols, phenols and carboxylic acids by 31P NMR
4.3.5 Global quantification of ketones by UV-visible spectroscopy
4.3.6 Final quantitative assessment
4.4 Conclusion
SPECIATION IN BIO-OIL UPGRADING PRODUCTS
CHAPTER 5. CHARACTERIZATION OF OXYGENATED COMPOUNDS IN UPGRADED BIO-OILS: A CRITICAL REVIEW 
5.1 Introduction
5.2 Generalities on upgraded bio-oils
5.2.1 Properties
5.2.2 Chemical functional groups
5.3 Characterization by one-dimensional gas chromatography
5.4 Characterization by two-dimensional gas chromatography
5.5 Discussion
5.6 Conclusion
CHAPTER 6. OXYGEN SPECIATION IN PARTIALLY UPGRADED BIO-OILS BY COMPREHENSIVE TWODIMENSIONAL GAS CHROMATOGRAPHY
6.1 Introduction
6.2 Experimental
6.2.1 Samples
6.2.2 GC×GC-FID setup
6.2.3 GC×GC-ToF/MS
6.2.4 Capillary columns
6.2.5 Data handling
6.3 Results and discussion
6.3.1 Investigating different column sets for oxygen speciation by GC×GC-FID
6.3.2 Identification by GC×GC-ToF/MS
6.3.3 Quantification by GC×GC-FID
6.4 Conclusion
CHAPTER 7. CHARACTERIZATION OF PHENOLIC COMPOUNDS IN PARTIALLY UPGRADED BIO-OILS BY SFCGC×GC
7.1 Introduction
7.2 Materials and methods
7.2.1 Samples
7.2.2 SFC-FID
7.2.3 Online GC×GC-FID
7.2.4 Offline GC×GC-FID and GC×GC-ToF/MS
7.2.5 SFC fractions transfer into the GC×GC system
7.2.6 Stationary phases
7.3 Results and discussion
7.3.1 SFC separation
7.3.2 Offline GC×GC analysis of SFC fractions
7.3.3 Online SFC-GC×GC analysis
7.4 Conclusion
ON ORTHOGONALITY IN GC×GC
CHAPTER 8. CONSIDERATIONS ON ORTHOGONALITY DUALITY IN COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY 
8.1 Introduction
8.2 Theory
8.3 Experimental section
8.3.1 Samples
8.3.2 GC×GC systems
8.4 Results and discussion
8.5 Conclusion
CHAPTER 9. REVERSAL OF ELUTION ORDER IN A SINGLE SECOND DIMENSION BY CHANGING THE FIRST COLUMNS NATURE IN COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY
9.1 Introduction
9.2 Experimental section
9.2.1 Samples
9.2.2 GC×GC systems
9.2.3 GC-FID conditions
9.3 Results and discussion
9.3.1 One column, two elution orders.
9.3.2 Influence of the first dimension on the second separation
9.3.3 van’t Hoff plots
9.3.4 Equations of the problem
9.3.5 Guidance on columns sets selection
9.4 Conclusion