Table Of Content

PLASTICS ADDITIVES This page intentionally left blank Plastics Additives Advanced Industrial Analysis By Jan C.J. Bart DSMResearch,TheNetherlands Amsterdam•Berlin•Oxford•Tokyo•Washington,DC ©2006,Theauthor. Allrightsreserved.Nopartofthisbookmaybereproduced,storedinaretrievalsystem, ortransmitted,inanyformorbyanymeans,withoutpriorwrittenpermissionfromthepublisher. TheauthorandthepublisherwishtothankAdriGeeve,DSMCoatingResinsB.V.(Zwolle,TheNetherlands)forproviding thecoverimage‘AnalyticalWebsite’. ISBN1-58603-533-9 LibraryofCongressControlNumber:2005931631 Publisher IOSPress NieuweHemweg6B 1013BGAmsterdam Netherlands fax:+31206870019 e-mail:[email protected] DistributorintheUKandIreland DistributorintheUSAandCanada GazelleBooks IOSPress,Inc. FalconHouse 4502RachaelManorDrive QueenSquare Fairfax,VA22032 LancasterLA11RN USA UnitedKingdom fax:+17033233668 fax:+44152463232 e-mail:[email protected] LEGALNOTICE Thepublisherisnotresponsiblefortheusewhichmightbemadeofthefollowinginformation. PRINTEDINTHENETHERLANDS Table of Contents Preface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xi AbouttheAuthor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xiii Acknowledgements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xv Chapter 1 In-PolymerSpectroscopicAnalysisofAdditives . . . . . . . . . . . . . . . . 1 1.1. DirectUltraviolet/VisibleSpectrophotometry . . . . . . . . . . . . . . . . 4 1.1.1. Vapour-phaseUltravioletAbsorptionSpectrometry . . . . . . . . . 10 1.2. Solid-stateVibrationalSpectroscopies . . . . . . . . . . . . . . . . . . . . 11 1.2.1. Mid-infraredSpectroscopicAnalysis . . . . . . . . . . . . . . . . . 14 1.2.2. Near-infraredSpectroscopy . . . . . . . . . . . . . . . . . . . . . . 34 1.2.3. RamanSpectroscopicTechniques. . . . . . . . . . . . . . . . . . . 52 1.3. PhotoacousticSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . 66 1.4. EmissionSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72 1.4.1. InfraredEmissionSpectroscopy . . . . . . . . . . . . . . . . . . . 72 1.4.2. MolecularFluorescenceSpectroscopy . . . . . . . . . . . . . . . . 75 1.4.3. PhosphorescenceSpectroscopy . . . . . . . . . . . . . . . . . . . . 81 1.4.4. Chemiluminescence . . . . . . . . . . . . . . . . . . . . . . . . . . 82 1.5. NuclearSpectroscopies . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94 1.5.1. Solid-stateNMRSpectroscopy . . . . . . . . . . . . . . . . . . . . 95 1.5.2. NuclearQuadrupoleResonance . . . . . . . . . . . . . . . . . . . . 110 1.5.3. ElectronSpinResonanceSpectroscopy . . . . . . . . . . . . . . . 112 1.5.4. MössbauerSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . 120 1.6. DielectricLossSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . 123 1.7. UltrasonicSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . 127 Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129 GeneralSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . 129 DirectUV/VISSpectrophotometry . . . . . . . . . . . . . . . . . . 129 InfraredSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . 129 Near-infraredSpectroscopy . . . . . . . . . . . . . . . . . . . . . . 130 RamanSpectroscopy. . . . . . . . . . . . . . . . . . . . . . . . . . 130 Photoacoustics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130 EmissionSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . 131 NMRSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . 131 ElectronSpinResonanceSpectroscopy . . . . . . . . . . . . . . . 131 DielectricSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . 131 PolymerCharacterisation . . . . . . . . . . . . . . . . . . . . . . . 131 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132 v vi TableofContents Chapter 2 Polymer/AdditiveAnalysisbyThermalMethods . . . . . . . . . . . . . . . . 155 2.1. ThermalAnalysisTechniques . . . . . . . . . . . . . . . . . . . . . . . . . 158 2.1.1. DifferentialScanningCalorimetry . . . . . . . . . . . . . . . . . . 163 2.1.2. DifferentialThermalAnalysis. . . . . . . . . . . . . . . . . . . . . 173 2.1.3. ThermogravimetricAnalysis . . . . . . . . . . . . . . . . . . . . . 175 2.1.4. SimultaneousThermalAnalysisMethods . . . . . . . . . . . . . . 189 2.1.5. (Multi)hyphenatedThermalAnalysisTechniques . . . . . . . . . . 192 2.1.6. ThermalMicroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . 209 2.1.7. Thermoluminescence . . . . . . . . . . . . . . . . . . . . . . . . . 213 2.2. PyrolysisTechniques. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 214 2.2.1. Pyrolysis–GasChromatography. . . . . . . . . . . . . . . . . . . . 222 2.2.2. Pyrolysis–MassSpectrometry . . . . . . . . . . . . . . . . . . . . . 235 2.2.3. Pyrolysis–GasChromatography–MassSpectrometry . . . . . . . . 244 2.2.4. Pyrolysis–FourierTransformInfraredSpectroscopy. . . . . . . . . 261 2.2.5. Pyrolysis–GasChromatography–FourierTransformInfrared Spectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 263 2.2.6. Pyrolysis–GasChromatography–AtomicEmissionDetection . . . 264 2.2.7. Temperature-programmedPyrolysis . . . . . . . . . . . . . . . . . 266 2.3. ThermalVolatilisationandDesorptionTechniques . . . . . . . . . . . . . 275 2.3.1. ThermalSeparationTechniques . . . . . . . . . . . . . . . . . . . . 278 2.3.2. DirectSolidSamplingTechniquesforGasChromatography . . . . 282 2.3.3. ThermalDesorption–MassSpectrometricTechniques. . . . . . . . 299 Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 300 ThermalAnalysis . . . . . . . . . . . . . . . . . . . . . . . . . . . 300 Pyrolysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 301 ThermalDesorption . . . . . . . . . . . . . . . . . . . . . . . . . . 301 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 301 Chapter 3 LasersinPolymer/AdditiveAnalysis . . . . . . . . . . . . . . . . . . . . . . . 325 3.1. Lasers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 325 3.2. LaserAblation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 331 3.2.1. LaserAblation–PlasmaSourceSpectrometry. . . . . . . . . . . . 335 3.3. LaserSpectroscopy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 341 3.3.1. Laser-inducedAtomicandMolecularFluorescence Spectrometry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 343 3.3.2. Laser-inducedBreakdownSpectroscopy . . . . . . . . . . . . . . . 346 3.4. LaserDesorption/IonisationMethods . . . . . . . . . . . . . . . . . . . . . 353 3.4.1. LaserDesorptionMassSpectrometry. . . . . . . . . . . . . . . . . 354 3.4.2. LaserIonisation . . . . . . . . . . . . . . . . . . . . . . . . . . . . 363 3.4.3. DecoupledLaserDesorption/Ionisation . . . . . . . . . . . . . . . 366 3.4.4. Matrix-assistedLaserDesorption/Ionisation . . . . . . . . . . . . . 374 3.4.5. LaserMicroprobeMassSpectrometry . . . . . . . . . . . . . . . . 381 3.5. LaserPyrolysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 388 Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 392 Lasers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 392 LaserAblation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 392 LaserSpectroscopy/Spectrometry. . . . . . . . . . . . . . . . . . . 392 Laser-inducedChemistry . . . . . . . . . . . . . . . . . . . . . . . 393 LaserSafety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 393 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 393 TableofContents vii Chapter 4 SurfaceAnalyticalTechniquesforPolymer/AdditiveFormulations . . . . . 403 4.1. ElectronSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 408 4.1.1. AugerElectronSpectroscopy . . . . . . . . . . . . . . . . . . . . . 409 4.1.2. X-rayPhotoelectronSpectroscopy . . . . . . . . . . . . . . . . . . 411 4.2. SurfaceMassSpectrometry . . . . . . . . . . . . . . . . . . . . . . . . . . 420 4.2.1. SecondaryIonMassSpectrometry . . . . . . . . . . . . . . . . . . 422 4.2.2. SecondaryNeutralMassSpectrometry . . . . . . . . . . . . . . . . 439 4.3. IonScatteringTechniques . . . . . . . . . . . . . . . . . . . . . . . . . . . 441 4.3.1. Low-energyIonScattering . . . . . . . . . . . . . . . . . . . . . . 443 4.3.2. RutherfordBackscatteringSpectroscopy . . . . . . . . . . . . . . . 444 Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 446 SurfaceCharacterisation . . . . . . . . . . . . . . . . . . . . . . . . 446 ElectronSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . 447 SurfaceMassSpectrometry . . . . . . . . . . . . . . . . . . . . . . 447 IonScatteringTechniques . . . . . . . . . . . . . . . . . . . . . . . 447 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 447 Chapter 5 MicroscopyandMicroanalysisofPolymer/AdditiveFormulations . . . . . . 455 5.1. ChemicalMicroanalysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . 458 5.2. MicroscopyandImagingTechniques . . . . . . . . . . . . . . . . . . . . . 460 5.3. LightMicroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 464 5.3.1. ConventionalOpticalMicroscopy . . . . . . . . . . . . . . . . . . 466 5.3.2. UltravioletMicroscopy . . . . . . . . . . . . . . . . . . . . . . . . 472 5.3.3. FluorescenceMicroscopy . . . . . . . . . . . . . . . . . . . . . . . 475 5.3.4. ConfocalandLaserMicroscopy . . . . . . . . . . . . . . . . . . . 478 5.4. ElectronMicroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 483 5.4.1. ScanningElectronMicroscopy . . . . . . . . . . . . . . . . . . . . 485 5.4.2. TransmissionElectronMicroscopy . . . . . . . . . . . . . . . . . . 494 5.4.3. AnalyticalElectronMicroscopy . . . . . . . . . . . . . . . . . . . 497 5.5. ScanningProbeMicroscopyTechniques . . . . . . . . . . . . . . . . . . . 501 5.5.1. AtomicForceMicroscopy . . . . . . . . . . . . . . . . . . . . . . . 504 5.5.2. Near-fieldScanningOpticalMicroscopy . . . . . . . . . . . . . . . 511 5.5.3. ScanningKelvinMicroscopy . . . . . . . . . . . . . . . . . . . . . 514 5.6. MicrospectroscopicImagingofAdditives . . . . . . . . . . . . . . . . . . 514 5.6.1. UV/VisibleMicrospectroscopy . . . . . . . . . . . . . . . . . . . . 519 5.6.2. InfraredMicrospectroscopyandImaging . . . . . . . . . . . . . . 521 5.6.3. Laser-RamanMicroprobeandMicroscopy. . . . . . . . . . . . . . 532 5.6.4. FluorescenceandLuminescenceImaging . . . . . . . . . . . . . . 541 5.7. MagneticResonanceImaging . . . . . . . . . . . . . . . . . . . . . . . . . 546 5.7.1. NuclearMagneticResonanceImaging . . . . . . . . . . . . . . . . 547 5.7.2. ElectronSpinResonanceImaging . . . . . . . . . . . . . . . . . . 555 5.8. X-rayMicroscopyandMicrospectroscopy . . . . . . . . . . . . . . . . . . 559 5.8.1. X-rayMicroradiography . . . . . . . . . . . . . . . . . . . . . . . . 560 5.8.2. ScanningX-rayMicroscopy. . . . . . . . . . . . . . . . . . . . . . 561 5.8.3. X-rayMicrofluorescence . . . . . . . . . . . . . . . . . . . . . . . 563 5.8.4. MicroX-rayPhotoelectronSpectroscopy . . . . . . . . . . . . . . 564 5.9. IonImagingofAdditives . . . . . . . . . . . . . . . . . . . . . . . . . . . 566 5.9.1. Laser-microprobeMapping . . . . . . . . . . . . . . . . . . . . . . 566 5.9.2. ImagingSecondaryIonMassSpectrometry . . . . . . . . . . . . . 567 viii TableofContents Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 573 LightMicroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . 573 ElectronMicroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . 573 ScanningProbeMicroscopy. . . . . . . . . . . . . . . . . . . . . . 574 Near-fieldOptics . . . . . . . . . . . . . . . . . . . . . . . . . . . . 574 MicrobeamAnalysis . . . . . . . . . . . . . . . . . . . . . . . . . . 574 Microspectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . 575 Imaging/ImageAnalysis . . . . . . . . . . . . . . . . . . . . . . . . 575 PolymerMicroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . 575 General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 576 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 576 Chapter 6 QuantitativeAnalysisofAdditivesinPolymers . . . . . . . . . . . . . . . . . 597 6.1. SamplingProceduresforQuantitativeAnalysisofPolymer/Additive Packages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 600 6.1.1. QuantitativeAnalysisofMineralFilledEngineeringPlastics . . . . 605 6.1.2. ReverseEngineeringofCuredRubberCompounds . . . . . . . . . 606 6.1.3. DeterminationofAdditiveBlendsinPolymers . . . . . . . . . . . 606 6.2. QuantitativeSolventandThermalExtraction . . . . . . . . . . . . . . . . 609 6.2.1. ExtractionandQuantificationofPolyolefinAdditives. . . . . . . . 613 6.2.2. SupercriticalFluidExtraction . . . . . . . . . . . . . . . . . . . . . 614 6.2.3. QuantificationofAntioxidantsinPolyolefins . . . . . . . . . . . . 615 6.2.4. DeterminationofPlasticisersbySolventandThermalExtraction . 619 6.2.5. Oil-extendedEPDM . . . . . . . . . . . . . . . . . . . . . . . . . . 623 6.2.6. MigrationRatesofPhthalateEstersfromSoftPVCProducts. . . . 624 6.3. QuantitativeChromatographicMethods . . . . . . . . . . . . . . . . . . . 624 6.3.1. QuantitativeGasChromatography . . . . . . . . . . . . . . . . . . 626 6.3.2. QuantitativeLiquidChromatography . . . . . . . . . . . . . . . . . 628 6.3.3. QuantitativeSupercriticalFluidChromatography . . . . . . . . . . 629 6.3.4. QuantitativeThin-layerChromatography . . . . . . . . . . . . . . 630 6.4. QuantitativeSpectroscopicTechniques . . . . . . . . . . . . . . . . . . . . 633 6.4.1. QuantitativeUltraviolet/VisibleSpectrophotometry . . . . . . . . . 637 6.4.2. QuantitativeFluorescenceSpectroscopy . . . . . . . . . . . . . . . 639 6.4.3. QuantitativeInfraredSpectroscopy . . . . . . . . . . . . . . . . . . 639 6.4.4. QuantitativeNear-infraredSpectroscopy . . . . . . . . . . . . . . . 644 6.4.5. QuantitativeRamanSpectroscopy . . . . . . . . . . . . . . . . . . 645 6.4.6. QuantitativeNuclearMagneticResonanceMethods. . . . . . . . . 646 6.5. QuantitativeMassSpectrometricTechniques . . . . . . . . . . . . . . . . 647 6.6. QuantitativeSurfaceAnalysisTechniques . . . . . . . . . . . . . . . . . . 651 6.7. QuantitativeMicroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . 653 Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 654 GeneralQuantitativeAnalysis. . . . . . . . . . . . . . . . . . . . . 654 Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 654 Chromatography . . . . . . . . . . . . . . . . . . . . . . . . . . . . 654 Spectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 655 MassSpectrometry. . . . . . . . . . . . . . . . . . . . . . . . . . . 655 SurfaceAnalysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . 655 ChemometricTechniques . . . . . . . . . . . . . . . . . . . . . . . 655 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 655 TableofContents ix Chapter 7 ProcessAnalytics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 663 7.1. In-processAnalysers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 667 7.2. ProcessSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 675 7.2.1. RemoteSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . 677 7.2.2. ProcessElectronicSpectroscopy . . . . . . . . . . . . . . . . . . . 679 7.2.3. Mid-infraredProcessAnalysisofPolymerFormulations . . . . . . 683 7.2.4. Near-infraredSpectroscopicProcessAnalysis . . . . . . . . . . . . 693 7.2.5. ProcessRamanSpectroscopy . . . . . . . . . . . . . . . . . . . . . 701 7.2.6. ProcessNuclearMagneticResonance . . . . . . . . . . . . . . . . 704 7.2.7. AcousticEmissionTechnology . . . . . . . . . . . . . . . . . . . . 716 7.2.8. Real-timeDielectricSpectroscopy . . . . . . . . . . . . . . . . . . 719 7.3. ProcessChromatography . . . . . . . . . . . . . . . . . . . . . . . . . . . 720 7.4. InSituElementalAnalysis. . . . . . . . . . . . . . . . . . . . . . . . . . . 721 Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 722 ProcessAnalyticalChemistry . . . . . . . . . . . . . . . . . . . . . 722 ProcessSpectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . 722 ProcessDataAnalysis . . . . . . . . . . . . . . . . . . . . . . . . . 723 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 723 Chapter 8 ModernAnalyticalMethodDevelopmentandValidation . . . . . . . . . . . 731 8.1. StatusofExistingMethodsforPolymer/AdditiveAnalysis . . . . . . . . . 732 8.2. In-polymerAdditiveAnalysis:MethodDevelopmentandOptimisation . . 732 8.3. CertifiedReferenceMaterials . . . . . . . . . . . . . . . . . . . . . . . . . 736 8.4. AnalyticalMethodValidationApproaches . . . . . . . . . . . . . . . . . . 746 8.4.1. AnalyticalPerformanceParameters. . . . . . . . . . . . . . . . . . 751 8.4.2. InterlaboratoryCollaborativeStudies . . . . . . . . . . . . . . . . . 755 8.4.3. ValidationofAntioxidantMigrationTesting . . . . . . . . . . . . . 757 8.5. TotalValidationProcess . . . . . . . . . . . . . . . . . . . . . . . . . . . . 757 8.5.1. Software/HardwareValidation/Qualification . . . . . . . . . . . . . 758 8.5.2. SystemSuitability . . . . . . . . . . . . . . . . . . . . . . . . . . . 760 8.6. RationalStep-by-stepMethodDevelopmentandValidationfor Polymer/AdditiveAnalysis . . . . . . . . . . . . . . . . . . . . . . . . . . 760 Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 762 MethodDevelopmentandValidation . . . . . . . . . . . . . . . . . 762 ReferenceMaterials . . . . . . . . . . . . . . . . . . . . . . . . . . 762 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 762 Appendix:ListofSymbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 767 AcronymsofTechniques . . . . . . . . . . . . . . . . . . . . . . . . . . . 767 ChemicalNomenclature . . . . . . . . . . . . . . . . . . . . . . . . . . . . 778 PolymersandProducts. . . . . . . . . . . . . . . . . . . . . . . . . 778 Additives/Chemicals . . . . . . . . . . . . . . . . . . . . . . . . . . 780 PhysicalandMathematicalSymbols . . . . . . . . . . . . . . . . . . . . . 785 PhysicalandMathematicalGreekSymbols . . . . . . . . . . . . . 789 GeneralAbbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 790 SubjectIndex . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 793 This page intentionally left blank

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Modern polymer/additive deformulation is essentially carried out according to three different approaches, in increasing order of sophistication, namely analysis of analytes separated from the polymer (typically an extract), of analytes and polymer in solution, or directly in-polymer (solid state or
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Modern polymer/additive deformulation is essentially carried out according to three different approaches, in increasing order of sophistication, namely analysis of analytes separated from the polymer (typically an extract), of analytes and polymer in solution, or directly in-polymer (solid state or

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