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New Concepts in Sorption Based Sample Preparation for Chromatography New concepts in sorption based sample preparation for chromatography Citation for published version (APA): Baltussen, H. A. (2000). New concepts in sorption based sample preparation for chromatography. Technische Universiteit Eindhoven. https://doi.org/10.6100/IR535092 DOI: 10.6100/IR535092 Document status and date: Published: 01/01/2000 Document Version: Publisher’s PDF, also known as Version of Record (includes final page, issue and volume numbers) Please check the document version of this publication: • A submitted manuscript is the version of the article upon submission and before peer-review. There can be important differences between the submitted version and the official published version of record. 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If the publication is distributed under the terms of Article 25fa of the Dutch Copyright Act, indicated by the “Taverne” license above, please follow below link for the End User Agreement: www.tue.nl/taverne Take down policy If you believe that this document breaches copyright please contact us at: [email protected] providing details and we will investigate your claim. Download date: 05. Oct. 2021 New Concepts in Sorption Based Sample Preparation for Chromatography New Concepts in Sorption Based Sample Preparation for Chromatography PROEFSCHRIFT ter verkrijging van de graad van doctor aan de Technische Universiteit Eindhoven, op gezag van de Rector Magnificus, prof.dr. M. Rem, voor een commissie aangewezen door het College voor Promoties in het openbaar te verdedigen op maandag 11 september 2000 om 16.00 uur door Henricus Antonius Baltussen geboren te Geldrop Dit proefschrift is goedgekeurd door de promotoren: prof.dr.ir. C.A.M.G. Cramers en prof.dr. P.J.F. Sandra aan Astrid aan mijn ouders CIP-DATA LIBRARY TECHNISCHE UNIVERSITEIT EINDHOVEN Baltussen, Henricus A. New concepts in sorption based sample preparation for chromatography / by Henricus A. Baltussen . - Eindhoven: Technische Universiteit Eindhoven, 2000. - Proefschrift. - ISBN 90-386-2971-0 NUGI 813 Trefwoorden: chromatografie / gas chromatografie ; mass spectrometrie / extractie / sporenanalyse Subject headings: chromatography / gas chromatography ; mass spectrometry / extraction / trace analysis Table of Contents Chapter 1 1 Introduction and Scope 7 1.1 General Introduction 7 1.2 Sample Preparation by Adsorption 8 1.3 Sample Preparation by Sorption 10 1.4 Scope of this Thesis 11 Chapter 2 2 State-of-the-art in Sample Preparation 13 2.1 Basic Concepts 13 2.1.1 Static Sampling 14 2.1.2 Dynamic Sampling 16 2.1.2.1 Definition of the Breakthrough Factor (b) 18 2.1.2.2 Differential Gaussian Breakthrough 19 2.1.2.3 Integrated Gaussian Breakthrough 21 2.1.2.4 Integrated Lövkvist Breakthrough 21 2.1.3 Classification of Extraction Approaches 23 2.2 Enrichment of Air and Gaseous Samples 23 2.2.1 Impringer and Denuder Techniques 24 2.2.2 Dynamic Adsorptive Extraction-Liquid Desorption 25 2.2.3 Dynamic Adsorptive Extraction-Thermal Desorption 28 2.3 Enrichment of Water and Liquid Samples 32 2.3.1 Dynamic Gas Phase Extraction (Purge and Trap) 33 2.3.2 Static Gas Phase Extraction (Headspace) 34 2.3.3 Liquid Phase Extraction (Liquid-Liquid Extraction) 34 2.3.4 Solid Phase Extraction 36 2.4 Enrichment of Soil, Sludge, Sediment and Solid Samples 41 2.4.1 Static and Dynamic Gas Phase Extraction 41 2.4.2 Dynamic Gas Phase Extraction (Thermal Desorption) 41 2.4.3 Liquid Extraction (Soxhlet) 42 2.4.4 Supercritical Fluid Extraction (SFE) 42 2.4.5 Accelerated Solvent Extraction (ASE) 43 2.4.6 Microwave Assisted Solvent Extraction (MASE) 44 1 New Concepts in Sorption Based Sample Preparation for Chromatography 2.4.7 Liquid Extraction (Micro Sonication) 44 2.5 Conclusions 45 References 47 Chapter 3 3 Sorptive Sample Preparation Methods 51 3.1 Principles of Sorption 51 3.2 Open Tubular Trapping 52 3.2.1 Gaseous Samples 53 3.2.2 Liquid Samples 54 3.3 Solid Phase Microextraction 55 3.4 Summary Sorptive Techniques – Advantages and Limitations 61 3.5 Conclusion 62 References 63 Chapter 4 4 Gum Phase Extraction for Gaseous Samples 65 4.1 Characteristics and Performance of Gum Phase Extraction (GPE) 65 4.1.1 Summary 65 4.1.2 Introduction 66 4.1.3 Theory 68 4.1.4 Experimental 71 4.1.4.1 Test Solutes 71 4.1.4.2 Sorbent and Adsorbent Cartridges 73 4.1.4.3 Instrumental Set-Up 74 4.1.4.4 Quantification 76 4.1.5 Results And Discussion 76 4.1.5.1 Standards 76 4.1.5.2 Determination of Organic Acids in Air 82 4.1.5.3 Determination of PAHs and Nitro-PAHs in Air 83 4.1.5.4 Headspace Sampling 86 4.1.6 Conclusion 88 4.2 Reactivity and Inertness for Sulfur Compounds 89 4.2.1 Summary 89 4.2.2 Introduction 89 4.2.3 Experimental 89 4.2.3.1 Thermal Desorption Cartridges 89 4.2.3.2 Experimental Set-Up 90 4.2.3.3 Standards 91 4.2.4 Results and Discussion 92 2 Table of Contents 4.2.5 Conclusion 95 4.3 GPE versus SPME - Analysis of Plant Volatiles 96 4.3.1 Summary 96 4.3.2 Experimental 96 4.3.2.1 Plant Material 96 4.3.2.2 Sampling Unit 96 4.3.2.3 Capillary GC-MS 97 4.3.2.4 Static Sampling 98 4.3.2.5 Dynamic Sampling 98 4.3.3 Results and Discussion 98 4.3.3.1 Evaluation of PDMS and PA Blank Levels 98 4.3.3.2 Static Sampling Using SPME with PDMS and PA Fibers 101 4.3.3.3 Dynamic Sampling on Cartridges Packed with Tenax and PDMS 103 4.3.4 Conclusion 105 4.4 Determination of Nicotine in Hospital Air 106 4.4.1 Summary 106 4.4.2 Introduction 106 4.4.3 Experimental 107 4.4.3.1 Sampling Cartridges and Air Sampling 107 4.4.3.2 Experimental Set-Up 107 4.4.4 Results and Discussion 108 4.4.4.1 System Evaluation and Smoke Characterization 108 4.4.4.2 Performance of PDMS Versus Adsorbents 109 4.4.4.3 Routine Monitoring 110 4.4.4.4 Filter Efficiency 112 4.4.5 Conclusion 113 4.5 Fast Analysis of PAHs in Air with Liquid Chromatography 114 4.5.1 Introduction 114 4.5.2 Theoretical Breakthrough 115 4.5.3 Experimental 116 4.5.3.1 Packed PDMS Traps 116 4.5.3.2 Experimental Set-Up 117 4.5.3.3 Air Sampling and On-Line LC Analysis 117 4.5.4 Results and Discussion 118 4.5.5 Conclusion 120 References 121 Chapter 5 5 Gum Phase Extraction for Liquid Samples 123 5.1 A Retention Model for Gum Phase Extraction of Aqueous Samples: Application to the Automated Analysis of Pesticides and PAHs in Water Samples 123 3 New Concepts in Sorption Based Sample Preparation for Chromatography 5.1.1 Summary 123 5.1.2 Introduction 124 5.1.3 Theory 126 5.1.4 Experimental 128 5.1.4.1 Test Solutes 128 5.1.4.2 PDMS Cartridges 129 5.1.4.3 Instrumental Set-Up 130 5.1.4.4 Sampling Program 131 5.1.5 Results and Discussions 132 5.1.6 Conclusion 136 5.2 Automated Sorptive Extraction-Thermal Desorption-GC-MS Analysis: Determination of Phenols in Water Samples 137 5.2.1 Summary 137 5.2.2 Introduction 137 5.2.3 Experimental 138 5.2.3.1 Chemicals and Materials 138 5.2.3.2 Instrumentation and Experimental Procedure 139 5.2.4 Results and Discussion 140 5.2.5 Conclusion 144 5.3 Capillary GC Determination of Amines in Aqueous Samples Using Sorptive Preconcentration on Polydimethylsiloxane and Polyacrylate Phases 145 5.3.1 Summary 145 5.3.2 Introduction 145 5.3.3 Experimental 147 5.3.3.1 Preparation of the Sorptive Phases 147 5.3.3.2 Experimental Set-Up 147 5.3.3.3 Experimental Procedure 148 5.3.4 Results and Discussion 148 5.3.4.1 Characterization of Blank Profiles 148 5.3.4.2 Determination of Amines in Tap Water 149 5.3.5 Conclusion 151 References 152 Chapter 6 6 Equilibrium Gum Phase Extraction 155 6.1 Summary 155 6.2 Introduction 155 6.3 Theory of Equilibrium Gum Phase Extraction 157 6.3.1 Calculation of Enrichment Factors 157 6.3.2 Influence of Pressure Drop 157 6.4 Experimental Section 159 4 Table of Contents 6.4.1 Thermal Desorption Cartridges 159 6.4.2 Experimental Set-Up 159 6.4.3 Chemical Standards 159 6.5 Results and Discussion 160 6.5.1 Prediction of Enrichment Factor 160 6.5.2 Equilibrium Sorption Profile 161 6.5.3 Displacement Effects 163 6.5.4 High Flow Sampling - Influence of Pressure Drop 164 6.5.5 EGPE Determination of Epichlorohydrin 164 6.5.6 Monitoring Ethylene Oxide in Air 165 6.6 Conclusion 167 References 168 Chapter 7 7 Stir Bar Sorptive Extraction 169 7.1 Study into the Equilibrium Mechanism Between Water and PDMS for Very Apolar Solutes: Adsorption or Sorption ? 169 7.1.1 Summary 169 7.1.2 Introduction 170 7.1.3 Experimental 171 7.1.3.1 Test Solutions 171 7.1.3.2 PDMS traps 171 7.1.3.3 Experimental Set-Up 172 7.1.3.4 Analytical Procedure 172 7.1.4 Results and Discussion 173 7.1.5 Conclusion 176 7.2 Stir Bar Sorptive Extraction (SBSE), a Novel Extraction Technique for Aqueous Samples.
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