This industrially relevant resource covers all established and emerging analytical methods for the deformulation of polymeric materials, with emphasis on the non-polymeric components.

• Each technique is evaluated on its technical and industrial merits.
• Emphasis is on understanding (principles and characteristics) and industrial applicability.

• Extensively illustrated throughout with over 200 figures, 400 tables, and 3,000 references.

  Autorentext

  Jan C.J. Bart (PhD Structural Chemistry, University of Amsterdam) is a senior scientist with broad interest in materials characterisation, heterogeneous catalysis and product development who spent an industrial carrier in R&D with Monsanto, Montedison and DSM Research in various countries. The author has held several teaching assignments and researched extensively in both academic and industrial areas; he authored over 250 scientific papers, including chapters in books. Dr Bart has acted as a Ramsay Memorial Fellow at the Universities of Leeds (Colour Chemistry) and Oxford (Material Science), a visiting scientist at Institut de Recherches sur la Catalyse (CNRS, Villeurbanne), and a Meyerhoff Visiting Professor at WIS (Rehovoth), and held an Invited Professorship at USTC (Hefei). He is currently a Full Professor of Industrial Chemistry at the University of Messina.
  He is also a member of the Royal Society of Chemistry, Royal Dutch Chemical Society, Society of Plastic Engineers and The Institute of Materials.

  Inhalt

  Foreword ix

  Preface xi

  About the Author xiii

  Acknowledgements xv

  Chapter 1 Introduction 1

  1.1 Additives 2

  1.1.1 Additive functionality 3

  1.2 Plastics formulations 5

  1.2.1 Supply forms 7

  1.2.2 Additive delivery 9

  1.3 Economic impact of polymer additives 9

  1.4 Analysis of plastics 11

  1.4.1 Regulations and standardisation 15

  1.4.2 Prior art 17

  1.4.3 Databases 19

  1.4.4 Scope 20

  1.4.5 Chapter overview 22

  1.5 Bibliography 23

  1.5.1 Plastics additives 23

  1.5.2 Processing technologies 23

  1.5.3 Instrumental analysis 23

  1.5.4 Polymer analysis 24

  1.5.5 Polymer/additive analysis 24

  1.6 References 24

  Chapter 2 Deformulation Principles 29

  2.1 Polymer identification 30

  2.2 Additive analysis of rubbers: 'Best Practice' 32

  2.3 Polymer extract analysis 42

  2.4 In situ polymer/additive analysis 46

  2.5 Class-specific polymer/additive analysis 47

  2.6 Bibliography 48

  2.6.1 Polymer identification 48

  2.6.2 Deformulation of rubbers 48

  2.6.3 Deformulation of polymers 48

  2.7 References 48

  Chapter 3 Sample Preparation Perspectives 51

  3.1 Solvents 54

  3.1.1 Polymer solubility criteria 55

  3.1.2 Solubility parameters 55

  3.1.3 Polymer solutions 56

  3.2 Extraction strategy 57

  3.3 Conventional extraction technologies 59

  3.3.1 Liquid-liquid extraction 60

  3.3.2 Liquid-solid extraction 60

  3.3.3 Classical solvent extractions of additives from polymers 61

  3.3.4 Sonication 75

  3.4 High-pressure solvent extraction methods 81

  3.4.1 Supercritical fluid technology 81

  3.4.2 Analytical SFE 85

  3.4.3 Subcritical water extraction 100

  3.4.4 Microwave technology 101

  3.4.5 Microwave-assisted extractions 104

  3.4.6 Pressurised fluid extraction 117

  3.5 Sorbent extraction 123

  3.5.1 Solid-phase extraction 124

  3.5.2 Solid-phase microextraction 129

  3.5.3 Stir bar sorptive extraction 133

  3.6 Methodological comparison of extraction methods 134

  3.6.1 Experimental comparisons 136

  3.6.2 Extraction selectivity 138

  3.6.3 'Nonextractable' additive analysis 140

  3.7 Polymer/additive dissolution methods 146

  3.8 Hydrolysis 152

  3.9 Bibliography 155

  3.9.1 Sampling and sample preparation 155

  3.9.2 Solvents/solubility 155

  3.9.3 Extraction methods 156

  3.10 References 156

  Chapter 4 Separation Techniques 171

  4.1 Analytical detectors 177

  4.2 Gas chromatography 181

  4.2.1 High-temperature gas chromatography 200

  4.2.2 Headspace gas chromatography 202

  4.3 Supercritical fluid chromatography 205

  4.4 Liquid chromatography techniques 217

  4.4.1 Planar chromatographies 218

  4.4.2 Column chromatographies 230

  4.5 Capillary electrophoretic techniques 273

  4.6 Bibliography 278

  4.6.1 General texts 278

  4.6.2 Detectors 279

  4.6.3 Gas chromatography 279

  4.6.4 Supercritical fluid chromatography 279

  4.6.5 Thin-layer chromatography 279

  4.6.6 Liquid chromatography 280

  4.6.7 Size-exclusion chromatography 280

  4.6.8 Ion chromatography 280

  4.6.9 Capillary electrophoretic techniques 280

  4.7 References 281

  Chapter 5 Polymer/Additive Analysis: The Spectroscopic Alternative 299

  5.1 Ultraviolet/visible spectrophotometry 302

  5.2 Infrared spectroscopy 311

  5.3 Luminescence spectroscopy 318

  5.4 High-resolution nuclear magnetic resonance spectroscopy 323

  5.4.1 Multidimensional NMR spectroscopy 336

  5.5 Bibliography 342

  5.5.1 General spectroscopy 342

  5.5.2 Ultraviolet/visible spectrophotometry 342

  5.5.3 Infrared spectroscopy 342

  5.5.4 Luminescence spectroscopy 342

  5.5.5 Nuclear magnetic resonance spectroscopy 342

  5.6 References 342

  Chapter 6 Organic Mass-Spectrometric Methods 349

  6.1 Basic instrumentation 351

  6.1.1 Inlet systems 352

  6.1.2 Modes of detection 353

  6.1.3 Mass resolution 354

  6.1.4 Isotope distributions 354

  6.1.5 Accurate mass measurements 355

  6.2 Ion sources 357

  6.2.1 Electron impact ionisation 360

  6.2.2 Chemical ionisation 362

  6.2.3 Metastable atom bombardment 367

  6.2.4 Fast atom bombardment 367

  6.2.5 Field ionisation 372

  6.2.6 Field desorption 374

  6.2.7 Thermospray ionisation 376

  6.2.8 Atmospheric pressure ionization techniques 378

  6.2.9 Desorption/ionisation methods 383

  6.2.10 Photoionisation techniques 385

  6.3 Mass analysers 386

  6.3.1 Sector analysers 387

  6.3.2 Quadrupole mass spectrometers 389

  6.3.3 Time-of-flight mass spectrometry 390

  6.3.4 Quadrupole ion trap 393

  6.3.5 Fourier-transform ion-cyclotron resonance mass spectrometry 395

  6.3.6 Tandem mass spectrometry 398

  6.4 Direct mass-spectrometric polymer compound analysis 407

  6.5 Ion mobility spectrometry 415

  6.6 Bibliography 417

  6.6.1 Mass spectrometry (General) 417

  6.6.2 Mass spectrometers 417

  6.6.3 Ionisation modes 417

  6.7 References 418

  Chapter 7 Multihyphenation and Multidimensionality in Polymer/Additive Analysis 425

  7.1 Precolumn hyphenation 428

  7.1.1 Chromatographic sampling methods 432

  7.2 Coupled sample preparation - spectroscopy/spectrometry 449

  7.3 Postcolumn hyphenation 452

  7.3.1 (Multi) hyphenated GC techniques 456

  7.3.2 (Multi) hyphenated SFC techniques 475

  7.3.3 (Multi) hyphenated HPLC techniques 489

  7.3.4 Hyphenated SEC techniques 527

  7.3.5 Hyphenated TLC techniques 530

  7.3.6 Hyphenated CE techniques 543

  7.4 Multidimensional chromatography 545

  7.4.1 Multidimensional gas chromatography 548

  7.4.2 Multidimensional supercritical fluid chromatography 550

  7.4.3 Multidimensional liquid chromatography 550

  7.4.4 Multidimensional thin-layer chromatography 558

  7.5 Multidimensional spectroscopy 560

  7.6 Bibliography 562

  7.6.1 General 562

  7.6.2 Multihyphenation and multidimensionality 563

  7.6.3 Precolumn hyphenation 563

  7.6.4 Postcolumn hyphenation 563

  7.6.5 Multidimensional chromatography 563

  7.6.6 Multidimensional spectroscopy 563

  7.7 References 564

  Chapter 8 Inorganic and Element Analytical Methods 585

  8.1 Element analytical protocols 587

  8.1.1 Element analytical pretreatment protocols 588

  8.1.2 Elemental analysis methods 589

  8.2 Sample destruction for classical elemental analysis 591

  8.2.1 Combustion analysis 593

  8.2.2 Wet matrix digestion 597

  8.2.3 Fusion methods 604

  8.3 Analytical atomic spectrometry 605

  8.3.1 Atomic absorption spectrometry 608

  8.3.2 Atomic emission spectrometry 613

  8.3.3 Atomic fluorescence spectrometry 624

  8.3.4 Direct spectrometric analysis of solid samples 625

  8.4 X-ray spectrometry 627

  8.4.1 X-ray f…