Compositional and Failure Analysis of Polymers A Practical Approach

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ISBN: 9780471625728 | 0471625728
Cover: Paperback
Copyright: 10/3/2000

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Intended as a practical guide for polymer technologists, engineers and analysts in the plastics, composites and rubber fields, this title describes a range of techniques and strategies for compositional and failure analysis of polymeric materials and products. Numerous examples illustrate the application of analytical methods for solving commonly encountered problems in the polymer industry. The reader is guided towards the most appropriate method of analysis and measurement and the most likely reasons for the failure. Areas covered include: * Migration and interaction of additives * Mechanical stress and stress cracking * Crazing and fracture * Residual stress and weld lines * Contamination and discoloration Numerous pedagogical methods, illustrative flow diagrams, figures and tables are used throughout the text to make it an invaluable guide to all analysts and polymer engineers in industrial or academic laboratories.

Preface

xxxi

About the Author

xxxiii

Acknowledgements

xxxv

Glossary

xxxvii

A Methodology for Solving Polymer Problems

(20)

Introduction

(3)

Flow Diagram for Solving Polymer Problems

(8)

Accurately Identify and Characterize the Failure

(4)

Are the Cause(s) Obvious and Few in Number?

(1)

Has this `Same' Product been Successfully Produced Previously?

(1)

Is there a Pattern to the Failure Location?

(1)

Is there a Trend in the Timing of the Problem?

(1)

Is this a Recurring Problem?

(2)

Are there Relationships between the Type of Failure and other Factors?

(1)

What Changes could have Affected the Failed Product When Compared to a Reference Sample?

(1)

Dealing with Special Problem Classes

(3)

Elusive Problems

(2)

Complex Problems

(1)

Subtle Problems

(1)

Initial Production Problems

(1)

Recurring Problems

(1)

Catastrophic or Major Problems

(1)

Product Life Cycle

(2)

Checklist and Worksheet for Organizing the Problem-Solving Process

(4)

References

(1)

Sampling and Sample Preparation

(16)

Introduction

(1)

Sampling

(1)

Sample Storage

(1)

Sample Conditioning

(1)

Sample Preparation

(13)

Grinding

(1)

Dissolution/Precipitation

(1)

Preparation of Polymer Films

(1)

Preparing Films for IR Analysis

(1)

Preparing Films for DSC/TG Analysis

(1)

Melt Pressing of Films

(1)

Film Casting

(2)

Introduction

(1)

Solvent

(1)

Film removal

(1)

Artifacts of solvent casting

(1)

Microtoming

(1)

Miscellaneous Sample Types

(1)

Intractable Samples

(1)

Brittle Thermoset Samples

(1)

Viscous Samples

(1)

Paints

(1)

Thin Films

(1)

Rubbers

(1)

Case Study

(1)

References

(1)

Microscopy of Polymers

(34)

Optical Microscopy Techniques

(18)

Introduction

(1)

Sample Illumination

(1)

Transmitted Illumination

(1)

Near-vertical Illumination

(1)

Incident Illumination

(1)

Grazing Incident Illumination

(1)

Coaxial Illumination

(1)

Dark-Field Illumination

(1)

Phase Contrast

(1)

Polarized Optical Microscopy

(7)

Sample Preparation

(1)

Microtoming

(1)

Microtome knife selection

(1)

Glass knives

(1)

General microtoming hints

(1)

Microtoming artifacts

(1)

Selection and preparation of the sample to be microtomed

(1)

Problem samples (irregular shaped and soft samples)

(1)

Problems encountered during microtoming

(1)

Trouble-shooting microtoming problems

(1)

Polishing

(1)

Hints for the polishing of samples

(1)

Polishing versus microtoming

(1)

Preparation of composites

(1)

Electron Microscopy

(5)

Scanning Electron Microscopy

(1)

Mounting SEM Samples

(1)

Charge Neutralization

(1)

Low-Voltage SEM

(1)

Transmission Electron Microscopy

(1)

Sample Preparation for TEM

(1)

Electron-Beam Damage

(1)

Special Microscopic Techniques

(5)

Thermomicroscopy

(1)

UV Microscopy

(1)

Atomic Force Microscopy

(2)

Practical Examples of the Uses of Microscopy in Polymer Analysis

(6)

Identification of Inhomogeneous Melts during Processing

(1)

Investigating Mould-Temperature Effects

(2)

Evaluation of the Extent of In-Mould Orientation

(1)

Examination of Fracture Surfaces

(1)

Identifying Crack-Initiation Sites

(1)

Examination of Rubber-Modified Polymers

(1)

Assessment of Oxidized Polymers

(1)

Microscopy of Fibres

(1)

Fibre Finish

(1)

Internal Texture of Fibres

(1)

Failure Analysis of Fibres

(1)

Microvoids in Aramid Fibres

(1)

PET Fibres

(1)

Beam-Induced Heating

(1)

Study of Residual Stresses

(1)

References

(1)

Fourier-Transform Infrared Spectroscopic Analysis Methods for Polymers

(36)

Introduction

(2)

IR Artifacts

(1)

Contaminant Peaks

(1)

Interference Fringes

(1)

Spectral Subtraction

(1)

FTIR Techniques

(11)

Transmission Analysis

(1)

ATR Analysis

(5)

Diffuse Reflectance IR (DRIFT)

(3)

Reflectance-Absorption FTIR

(1)

Photoacoustic FTIR

(1)

FTIR Microspectroscopy

(1)

Introduction

(2)

Embedding Media

(1)

FTIR Mapping Techniques

(1)

Reflectance ETIR Microscopy

(1)

Thermomicroscopy-FTIR

(1)

Special IR Techniques

(3)

NIR Analysis

(2)

Raman-FTIR

(1)

Sample Preparation

(6)

Compression Moulding of Thin Films

(3)

KBr Preparation

(1)

Sample Supports

(2)

Pellets

(1)

Abrasion Method

(1)

FTIR Analysis of Difficult Sample Forms

(8)

Ground Polymers or Inorganic Ash

(1)

Polymer Fibres

(1)

Carbon-Filled Samples

(1)

Thin Films on Reflective Substrates

(1)

Irregularly Shaped Samples

(1)

Polymer Foams

(1)

Polymer Composites

(1)

Clear, Highly Elastomeric Samples

(2)

Thick Viscous Samples

100

(1)

Microsamples

100

(1)

Paints

100

(1)

Samples with Suspected Surface Contamination

101

(1)

Multilayer Samples

101

(1)

Interpreting and Validating FTIR Data

101

(4)

Introduction

101

(2)

Steps Involved in PVC and PVDC Identification

103

(1)

IR Identification of Styrenics

104

(1)

Distinguishing between Polyamides and Polyurethanes

104

(1)

Nylon Analysis

104

(1)

Derivatization Techniques

105

(2)

An Example of Derivatization

105

(1)

References

106

(1)

Thermal Analysis of Polymers

107

(40)

Introduction

107

(1)

Differential Scanning Calorimetry

108

(21)

Introduction

108

(1)

Representative Sampling

109

(1)

Sample Preparation for DSC

109

(1)

Effect of Sample Mass and Heating Rate

110

(1)

Advanced DSC Techniques

110

(1)

Information that can be Obtained by DSC Analysis

110

(1)

Thermal History

110

(2)

Melting Point

112

(1)

Glass Transition Temperature

113

(2)

Polymer Crystallinity

115

(1)

Crystallization Behaviour

116

(1)

Crystallization Kinetics

117

(1)

Cooling Rate of a Polymer Component

117

(1)

Physical Ageing

117

(2)

Detecting the Presence of Regrind

119

(1)

Evaluating Heat Ageing of Semicrystalline Polymers

119

(2)

Evaluating Heat Ageing of Amorphous Polymers

121

(1)

Evaluating Effects of Solvents on Amorphous Polymers

122

(1)

Unusual DSC Features

122

(1)

Cold Crystallization

123

(1)

Water-Related Phenomena

124

(1)

Secondary Melting Peaks

124

(3)

Unexpected Exothermic Deviations

127

(1)

DSC Behaviour of Common Polymers

127

(1)

Amorphous Polymers

127

(1)

PET

127

(1)

PPS

128

(1)

PBT

128

(1)

Nylon 6

128

(1)

Dynamic Mechanical Thermal Analysis

129

(2)

Dynamic Mechanical Rheological Testing

131

(1)

Thermomechanical Analysis

132

(1)

Glass Transition Temperature and its Determination

133

(5)

Introduction

133

(1)

Determining Tg

133

(5)

Thermogravimetry

138

(7)

Introduction

138

(1)

Isothermal TG

138

(1)

Important Experimental Factors

139

(2)

High-Resolution TG

141

(1)

TG---FTIR

141

(3)

Limitations of TG-FTIR

144

(1)

TG MS

144

(1)

Thermal Volatilization Analysis

145

(2)

References

145

(2)

Identification and Analysis of Polymers

147

(46)

Introduction

147

(6)

Density Measurement

147

(2)

Flammability Testing

149

(1)

Thermal Analysis and FTIR Spectroscopic Methods

150

(1)

Chemical Equivalency

151

(1)

Solubility Testing

151

(1)

Structural Information on Polymers

151

(2)

Molecular Weight Measurement

153

(1)

Examples of Analytical Techniques used for Common Polymers

153

(40)

ABS Analysis

153

(1)

Introduction

153

(1)

Determining the Rubber Content of ABS

154

(1)

Analysis of Weathered ABS

155

(1)

Epoxy Analysis

156

(1)

Introduction

156

(1)

FTIR and NMR Spectroscopies

157

(1)

High Performance Liquid Chromatography

157

(1)

UV Analysis

157

(1)

EVA Analysis

158

(1)

FTIR Spectroscopy

158

(1)

Thermogravimetry

158

(1)

TG-Titrimetry

159

(2)

TG MS

161

(1)

Thermal Volatilization Analysis

161

(1)

UV Spectrophotometry

161

(1)

Fluoropolymer Analysis

161

(1)

HIPS Analysis

162

(1)

Determining the Polybutadiene Content of HIPS

163

(2)

Liquid Crystal Polymer Analysis

165

(1)

Nylon Analysis

165

(1)

FTIR Spectroscopy

165

(1)

DSC

166

(1)

PBT Analysis

166

(1)

DSC

166

(1)

MW Determination

167

(1)

Polycarbonate Analysis

167

(1)

PE Analysis

168

(1)

FTIR Spectroscopy

168

(1)

Fractionation

169

(1)

PEEK Analysis

170

(1)

DSC

170

(1)

Determining Crystallinity

170

(1)

Crystallization Behaviour

171

(1)

Determining the Glass Transition

172

(1)

Thermal Degradation of PEEK

172

(1)

PET Analysis

172

(1)

Phenolic Resin Analysis

173

(1)

FTIR Spectroscopy

173

(1)

Chromatographic Techniques

174

(1)

Pyrolysis-GC-MS

174

(1)

TG-MS

174

(1)

PMMA Analysis

175

(1)

Polysulfone Analysis

175

(1)

PP Analysis

175

(1)

FTIR Spectroscopy

175

(1)

DSC

176

(1)

MW Fractionation

176

(1)

Analysing PP Copolymers

176

(1)

PPO Analysis

177

(1)

PPS analysis

177

(2)

PU Analysis

179

(1)

Introduction

179

(1)

Compositional Analysis of PUs by FTIR Spectroscopy

180

(2)

Sample Preparation for FTIR Spectroscopy

182

(1)

Identifying the Acid in the Ester Portion of PU

182

(1)

Determing NCO Content

182

(1)

Analysis of Hydrolytic Breakdown Products

183

(1)

DSC Analysis

184

(1)

Pyrolysis Methods

184

(1)

PVC Analysis

184

(1)

FTIR Spectroscopy

184

(1)

Analysis of Plasticizers

185

(1)

Determination of Impact Modifiers

185

(1)

MW Determination

186

(1)

Determination of Crystallinity

186

(1)

Determining the Glass Transition Temperature

187

(1)

Degree of Fusion of PVC

187

(1)

Degradation of PVC

187

(1)

SAN Analysis

188

(1)

Silicone Rubber Analysis

188

(1)

Thermoplastic PU Elastomer Analysis

188

(1)

Unsaturated Polyester Resin Analysis

189

(1)

References

189

(4)

Analysis of Blends, Copolymers and Oligomers

193

(22)

Polymer Blends

193

(8)

Introduction

193

(1)

Miscibility of Blends

194

(1)

Immiscible Blends

195

(1)

Compatibilization

196

(1)

Interpenetrating Networks

196

(1)

Determination of the Blend Miscibility and Blend Ratio

196

(1)

Analysis of Phase Dispersion in Polymer Blends

196

(2)

Examples of Techniques for Determining Blend Composition

198

(1)

Composition of LLDPE/LDPE Blends by DSC

198

(1)

Composition of Nory1™ Blends by DSC

199

(1)

Composition of Nory1™ Blends by Pyrolysis-Gas Chromatography

200

(1)

Copolymers

201

(5)

Introduction

201

(2)

Copolymer Analysis

203

(1)

Analysis of Block Copolymers

203

(2)

Microscopy of Copolymers

205

(1)

FTIR Spectroscopic Analysis of Copolymers

205

(1)

Oligomers

206

(9)

Introduction

206

(1)

Analysis Methods

207

(1)

HPLC

207

(1)

Supercritical Fluid Chromatography

208

(1)

Laser-Desorption/Fourier-Transform Mass Spectrometry

208

(1)

Oligomers in HDPE

208

(2)

Oligomers in PET

210

(2)

Oligomers in Silicone Polymers

212

(1)

Oligomers in PMMA

213

(1)

References

213

(2)

Identification and Analysis of Thermoset Elastomers

215

(15)

Thermogravimeny

215

(7)

FTIR Spectroscopic Analysis of Carbon-Filled Rubbers

222

(1)

Sample Preparation for FTIR Spectroscopy

222

(1)

Rubber Identification by Pyrolysis Methods

223

(1)

Pyrolysis-IR Spectroscopy

223

(1)

Pyrolysis-GC

223

(1)

Pyrolysis-GC-MS

223

(1)

Pyrolysis-MS

224

(1)

Analysis of Specific Rubber Types

224

(6)

SBR Analysis

224

(1)

PB Analysis

225

(1)

NBR Analysis

225

(1)

Polychloroprene Analysis

226

(1)

EPDM Analysis

226

(2)

Thermoplastic Elastomer Analysis

228

(1)

References

228

(2)

Analysis of `Difficult' or Intractable Polymer Samples

230

(10)

Introduction

230

(1)

FTIR Spectroscopic Techniques for Difficult Samples

230

(3)

DRIFT Analysis of Intractable Materials

231

(1)

Abrasion-DRIFT Analysis

231

(1)

Photoacoustic FTIR Spectroscopy

232

(1)

Pyrolysis of Intractable Samples

233

(3)

Pyrolysis of Small Samples

233

(1)

Manipulation of Pyrolytic Oils

234

(1)

Pyrolysis-IR Spectroscopy

234

(1)

Pyrolysis-GC-FTIR Spectroscopy

234

(1)

Rubber Pyrolysis

234

(2)

Vacuum Pyrolysis

236

(1)

Pyrolysis in the MS Ion Source

236

(1)

Thermogravimetry

236

(1)

Laser-Desorption Fourier-Transform Mass Spectrometry

237

(3)

References

239

(1)

Analysis of Additives in Polymers and Elastomers

240

(30)

Introduction

240

(1)

Grinding

241

(1)

Additive Extraction

242

(6)

Soxhlet Extraction

243

(1)

Soxtec™ Extraction

243

(1)

Reflux Extraction

243

(1)

Solvent Extraction of Polymer Films

244

(1)

Ultrasonic Extraction

244

(1)

Microwave-Assisted Extraction

245

(1)

Supercritical Fluid Extraction

246

(2)

Analysis Methods

248

(11)

UV Spectroscopic Analysis of Additives

248

(1)

IR Spectroscopic Analysis of Additives

248

(1)

GC Analysis of Additives

249

(1)

HPLC Analysis of Additives

249

(2)

GC-MS Analysis of Additives

251

(1)

SEC-GC-MS Analysis of Additives

252

(1)

Supercritical Fluid Chromatography Analysis of Additives

252

(2)

SFC-FTIR Spectroscopic Analysis of Additives

254

(1)

In situ Additive Detection in Polymers

254

(1)

XRF Analysis

254

(2)

Examples of the Use of XRF for Additive Analysis

256

(1)

Common elements

256

(1)

Uncommon elements

257

(1)

Specific element combinations

257

(1)

Important Considerations in XRF Analysis

258

(1)

Sample preparation

258

(1)

Experimental technique

258

(1)

Spectral interference

259

(1)

In situ Additive Analysis in Rubbers

259

(1)

Miscellaneous Examples of Additive Analysis Methods

260

(10)

Unknown Additive Analysis

260

(1)

Antistatic Additive Analysis

261

(1)

Thioester Additive Analysis

261

(1)

Oligomeric (`Non-Extractable') Additive Analysis

261

(1)

Carbon Black Determination

262

(2)

Filler Analysis

264

(1)

Furnace Ashing

264

(2)

Filler Content Quantification

266

(1)

Filler/Pigment Content Determination of Polyamides and Polyesters

266

(1)

Ash Analysis by FTIR Spectroscopy

267

(1)

Determination of Fibre Content and Distribution in Glass-Reinforced Composites

268

(1)

References

268

(2)

Analysis of Contaminants and Inclusions in Polymers

270

(34)

Introduction

270

(1)

Classes of Typical Contamination

271

(9)

Black Specks

271

(4)

Cellulosic Contamination

275

(1)

Metal Contamination

275

(2)

Polymeric Contamination

277

(1)

Additive Contamination

278

(1)

Contamination From Storage and Shipping Containers

279

(1)

Chemical Contamination

279

(1)

Miscellaneous Sources of Contamination

280

(1)

Techniques for Analysis of Contamination

280

(8)

Optical Microscopy

280

(1)

FTIR Microscopy

281

(1)

EDAX (X-Ray Microanalysis)

282

(1)

ESCA

283

(1)

Micro-XRF

283

(1)

Pyrolysis-GC

283

(1)

Thermogravimetry

284

(1)

TG-GC-MS

284

(1)

TP-SIP-MS

285

(1)

TOF-SIMS

285

(1)

Screening Polymer Batches for Contamination

286

(2)

Gel Particles and other Inclusions

288

(16)

Introduction

288

(3)

Gels in PE

291

(2)

Gels in PP

293

(1)

Gels in PVC

294

(1)

Oxidized Particles in Polymers

294

(1)

Gels due to Additives

295

(1)

Contamination-Related Gels

295

(1)

Foreign Polymer Gels

296

(1)

Analysis of Gel Imperfections

296

(1)

Polarized-Light Examination

296

(1)

Hot-Stage Microscopy

296

(2)

FTIR Microscopy

298

(2)

DSC Analysis

300

(1)

Micro-Ashing

300

(2)

Quantitying Gel Defects

302

(1)

References

302

(2)

Mechanical Failure Mechanisms of Polymers

304

(59)

Introduction

304

(6)

Tensile Failure

310

(1)

Shear Failure

310

(1)

Compressive Failure

311

(1)

Crazing

311

(2)

Introduction

311

(1)

Crazing in Rubber-Modified Polymers

311

(1)

Analysis of Crazing

312

(1)

Shear Banding

313

(2)

Introduction

313

(1)

Analysis of Shear Banding

314

(1)

Shear Deformation (Banding) versus Crazing

314

(1)

Creep

315

(2)

Introduction

315

(1)

Measuring Creep

316

(1)

Fatigue Failure

317

(7)

Introduction

317

(3)

Measuring Fatigue Resistance

320

(1)

Examples of Fatigue Behavior in Different Polymers

321

(1)

Fatigue of Polyacetal

321

(1)

Fatigue of Toughened Styrenic Polymers

321

(1)

Fatigue of Rubbers

321

(1)

Fatigue of Nylon

322

(1)

Fatigue of Short-Fibre-Reinforced Plastics

322

(1)

Fatigue of Continuous-Fibre Composites

322

(1)

Analysing Fatigue Fracture

323

(1)

Impact Fracture

324

(6)

Introduction

324

(1)

Measuring Impact Strength

325

(2)

Notch-Sensitivity

327

(1)

Temperature Sensitivity

328

(2)

Physical Ageing

330

(3)

Introduction

330

(2)

Common Polymers which Undergo Physical Ageing

332

(1)

PVC

332

(1)

PET

332

(1)

PPO

332

(1)

Physical Ageing of Rubber-Modified Glassy Polymers

333

(1)

Analysis of Physical Ageing

333

(1)

Failure Due to Temperature Effects

333

(3)

Maximum- and Minimum-Use Temperatures

333

(2)

Temperature Sensitivity of Creep Modulus

335

(1)

Thermal Shock

335

(1)

Failure Due to Improper Processing

336

(3)

Problems due to Excessive in-Mould Orientation

336

(1)

Melting and Moulding Temperatures

336

(1)

Was the Correct Mould Temperature Used?

337

(1)

Use of Regrind

338

(1)

General Examples of Polymer Failure

339

(13)

PVC

339

(1)

Brittle Failure in PVC

339

(2)

Thermal Degradation of PVC

341

(1)

Physical Ageing of PVC

341

(1)

Annealing

342

(1)

Impact Strength

342

(1)

Strain-Rate Effects on PVC

343

(1)

Embrittlement of PVC by Loss of Plasticizer

343

(1)

Stress Concentrations

344

(1)

Polycarbonate

344

(1)

Introduction

344

(1)

MW Reduction

345

(1)

Processing Conditions

345

(1)

Solvent-Induced Crystallization

346

(1)

Structural Flaws and Surface Stresses

347

(1)

Nylon

347

(1)

PET

347

(1)

PBT

348

(1)

PPS

348

(1)

Polyacetal

349

(1)

Impact-Modified Polymers

349

(1)

Epoxy Resins

350

(1)

Unsaturated Polyesters

350

(1)

Polyetherimide

350

(1)

Polysulfones

350

(1)

Thermoplastic Polyurethanes

351

(1)

PTFE

351

(1)

Failure of Short-Fibre-Glass-Reinforced Thermoplastics

351

(1)

Failure of Medical Plastics

352

(1)

Failure of Polymers and Elastomers by Explosive Decompression

352

(7)

Polymers Susceptible to ED Damage

355

(1)

Nature of ED Damage

356

(3)

Failure Analysis by Fractography

359

(4)

References

361

(2)

Chemical Attack of Polymers

363

(34)

Introduction

363

(2)

Factors Determining Chemical Resistance

365

(1)

Types of Chemical Attack

365

(26)

Hydrolytic Degradation of Polymers

365

(1)

Introduction

365

(2)

Hydrolysis of Poly(ethylene Terephthalate)

367

(1)

Hydrolysis of Polycarbonate

368

(1)

Hydrolysis of Polyacetals

369

(3)

Hydrolysis of Polyurethanes

372

(1)

Hydrolysis of Polyethersulfones

372

(1)

Hydrolysis of Thermosets

372

(1)

Hydrothermal Degradation of Composites

373

(1)

Hydrolysis During Steam Autoclaving of Polymers

373

(1)

Acid and Alkaline Attack

374

(1)

Introduction

374

(1)

Additives and Residues from Manufacturing Operations

374

(1)

Environmental Exposure

374

(1)

In vivo Situations

375

(1)

By-Products of Degradation

375

(1)

Service Use

375

(3)

Analysing for Acid Attack

378

(1)

Acid-Catalysed Hydrolysis

379

(2)

Alkaline Attack

381

(1)

Chemical Degradation by Strong Oxidizing Liquids

381

(1)

Ester-Interchange and Transesterification Reactions

382

(1)

Aminolysis

382

(3)

Rubber Degradation by Chloramines

385

(1)

Solvent Attack

385

(2)

Solvation

387

(1)

Salt Solutions

388

(1)

Catalysed Chemical Degradation

388

(1)

Microbial Chemical Degradation

389

(2)

Analysis Methods for Assessing Chemical Degradation

391

(4)

Introduction

391

(1)

Mechanical Tests

392

(1)

Swelling Tests

392

(1)

DMTA

393

(1)

Headspace Analysis

393

(1)

FTIR Spectroscopic Analysis

393

(1)

EDAX

394

(1)

Case Study

395

(2)

References

395

(2)

Oxidative Degradation of Polymers

397

(52)

Introduction

397

(13)

Factors Affecting Polymer Oxidation

401

(1)

Temperature

401

(1)

Branching (Tertiary Hydrogen Atoms)

402

(1)

Oxygen Diffusion

402

(1)

Polymer Unsaturation

403

(1)

Catalyst Residues

403

(1)

Stress

404

(1)

Effect of Oxidation on Polymer Properties

404

(1)

Molecular Weight

404

(1)

Mechanical Properties

405

(1)

Other Properties

406

(1)

Heterogeneous Oxidation

406

(1)

Metal-Catalysed Oxidation

406

(2)

Processing Degradation

408

(2)

Accelerated Ageing Techniques

410

(4)

Oven Ageing

411

(1)

Assessing Processing Degradation by Multipass Extrusion

411

(1)

Extrapolation of Oxidative Ageing Data

412

(1)

Some Problems with Arrhenius Extrapolations

412

(1)

Discontinuities in extrapolation plots due to polymer transitions

412

(1)

Temperature fluctuations in ovens used for accelerated ageing

413

(1)

Changes in `cage' effect with temperature

413

(1)

Sample non-uniformity

413

(1)

Differences in antioxidant solubility below and above the polymer Tm

413

(1)

Stress relaxation

413

(1)

Testing Methods

414

(35)

Melt-Flow Index

414

(1)

Residence-Time Melt-Flow Index

415

(1)

IR Spectroscopic Methods

416

(1)

Carbonyl Index

417

(1)

Limitations of Carbonyl Measurements

417

(1)

Derivation of Carbonyl and Hydroxyl Groups

418

(1)

Differential Scanning Calorimetry

419

(1)

Oxidative Induction Time (OIT)

420

(1)

Introduction

420

(2)

Limitations of the OIT Method

422

(2)

Extrapolation of OIT Data

424

(1)

Thermogravimetric Analysis

424

(1)

Gel Content of Oxidized Polymers

424

(2)

ESR Spectroscopy

426

(1)

XPS

426

(1)

Oxygen Uptake

426

(1)

Introduction

426

(1)

Shape of Oxygen-Uptake Curve

427

(1)

Constant-Volume and Constant-Pressure Instruments

428

(1)

Manometers/Manual Apparatus

428

(2)

Limitations of Oxygen Uptake

430

(1)

Hydroperoxide Detection

431

(1)

Introduction

431

(1)

Iodometric Method

432

(2)

Ferric Thiocyanate Method

434

(1)

Infrared Spectroscopic Methods

435

(1)

Chemiluminescence (CL)

435

(3)

Hydroperoxide Concentration by CL

438

(1)

Staining Techniques

439

(4)

References

443

(6)

Failure of Fibre-Reinforced Composites

449

(33)

Introduction

449

(3)

Fibre Adhesion in Composites

452

(2)

Analysis of Fibre Adhesion in Composites

453

(1)

Failure of Composites due to Manufacturing and Cure-Related Factors

454

(4)

Impurities in Commercial Thermosetting Resins

454

(2)

Advancement of Prepreg Resin During Storage

456

(1)

Distribution of Curing Agents

456

(1)

Premature Curing

456

(1)

Incomplete Curing

457

(1)

Cure Progression

458

(1)

Failure Behaviour of Composites

458

(13)

Types of Failure Mechanisms of Composites

459

(1)

De-bonding

459

(1)

Interlaminar Failure

459

(2)

Fibre Buckling

461

(1)

Fibre Pull-Out

461

(1)

Fibre Breakage

461

(1)

Cracking of Composites

462

(1)

Micro-cracking of Composites

462

(1)

Types of Loading Modes to which Composites are Subjected

463

(1)

Tensile Loading Failures

463

(1)

Compressive Loading Failures

464

(2)

Shear Loading Failures

466

(1)

Stress Rupture of Composites

467

(1)

Impact Damage of Composites

467

(2)

Fatigue Failure of Composites

469

(2)

Heat generation during fatigue

471

(1)

Creep of Composites

471

(1)

Failure of Composites due to Thermal Effects

471

(2)

Effects of Moisture on Composites

473

(1)

Hygrothermal Degradation of Composites

473

(1)

Analysis of Hygrothermal Degradation Problems

474

(1)

Chemical Attack on Composites

474

(1)

Environmental Stress Cracking

474

(1)

Oxidative Degradation

475

(1)

Photo-Oxidative Degradation of Fibre Reinforcements

475

(1)

Radiation Degradation of Composites

476

(1)

Failure Testing of Composites

476

(1)

Detecting Cracking in Composites

476

(1)

Fractography of Composites

477

(5)

Introduction

477

(1)

Specific Fractographic Examples

478

(1)

Tensile Failure

478

(1)

Mode-I Tension

479

(1)

Mode-II Shear

479

(1)

Quantifying the Fracture Surface

480

(1)

References

480

(2)

Problems Related to Additive in Polymers

482

(36)

Introduction

482

(1)

Blooming

482

(5)

Analysis

486

(1)

Sublimation

487

(1)

Analysis

488

(1)

Plateout

488

(1)

Analysis

489

(1)

Die Drool

489

(1)

Bleeding

490

(1)

Analysis

490

(1)

Additive Migration

491

(1)

Analysis

492

(1)

Additive Interactions

492

(4)

Antagonistic Additive Interactions

492

(3)

Physical Adsorption of Additives

495

(1)

Additive Decomposition

496

(6)

Thermal Decomposition of Nucleating Agents

496

(1)

Slip-Additive Degradation

497

(1)

Flame Retardants

497

(1)

Hindered-Amine Light Stabilizers

498

(1)

Pigments

498

(1)

Thermal Stability and Photostability of Pigments

498

(2)

Analysis of Pigments

500

(1)

Loss of Water of Hydration and Volatiles Formation

500

(1)

Pigment-Polymer Reactions

501

(1)

Additive-Induced Polymer Decomposition

502

(5)

Thermal Oxidation

502

(2)

Analysis

504

(1)

Photo-Oxidation

504

(1)

Analysis to Determine Catalytic Activity of TiO2 Pigments

505

(2)

Chain Cleavage by Nucleating Agents

507

(1)

Additive Dispersion Problems

507

(7)

Analysis

514

(1)

Effect of Additives on the Polymers Mechanical Properties

514

(1)

Pigment-Induced Distortion

515

(1)

Abrasion

516

(2)

References

516

(2)

Weathering of Polymers

518

(28)

Introduction

518

(4)

Preliminary Investigations

522

(1)

Detail the Problem

522

(1)

Sample Selection

522

(1)

Visual/Microscopic Inspection

523

(1)

Polymer Identification

523

(1)

Case Studies

523

(13)

PVC Window Frames and Sidings

523

(1)

Background

523

(3)

Decision Tree and Testing

526

(1)

Impact strength

526

(1)

FTIR spectroscopic analysis

527

(3)

Miscellaneous tests

530

(1)

Polyolefin Garden Furniture and Milk Crates

530

(1)

Background

530

(1)

Decision Tree and PP Testing

531

(5)

Decision Tree and HDPE Testing

536

(1)

Problems with Other Polymer Types and Applications

536

(5)

PP/EPDM Fenders

536

(1)

PMMA Glazing

537

(1)

537

(1)

Acrylonitrile-Butadiene-Styrene Housings

538

(1)

Styrene-Acrylonitrile Car Grillls

539

(1)

Polyester/Glass Composite (`Fibreglass') Sheeting

539

(1)

Acrylic Surface Coatings

540

(1)

Polymer Weatherability Assessment (Accelerated Weathering)

541

(5)

Xenon-Arc Devices

542

(1)

The QUV Weathering Chamber

543

(1)

The SEPAP Weathering Chamber

543

(1)

Pitfalls in Accelerated Weathering Testing

544

(1)

References

545

(1)

Environmental Stress Cracking of Polymers

546

(41)

Introduction

546

(3)

ESC Mechanisms

549

(5)

Amorphous Plastics

549

(1)

Semicrystalline Polymers

550

(1)

The Stress Factor

550

(1)

Stress-Cracking Agents

550

(1)

Direct Stress Cracking (by Sorption)

551

(1)

Indirect Stress Cracking (by Desorption)

552

(2)

Degradative Stress Cracking

554

(1)

Special Applications where ESC is likely to Occur

554

(2)

Adhesive Bonding and Solvent Welding

554

(1)

Contact between Dissimilar Polymers

554

(1)

Welded Assemblies

555

(1)

Metal Inserts

555

(1)

Lubricated/Moving Parts

556

(1)

Testing Methods to Determine ESC Resistance

556

(5)

Constant-Deformation Test

556

(1)

Ball-Indentation Test (ISO-4600)

556

(1)

Bent-Strip Test Method (ISO-4599)

557

(1)

Polyolefin Bent-Strip Test (ASTM-D1693)

558

(1)

Constant-Load Test (ASTM-5397)

559

(1)

Spiral-Cone Method

560

(1)

Bottle ESCR Test

561

(1)

Surface-Tension and Solubility-Parameter Effects

561

(2)

Predicting ESC based on Solubility Parameters

562

(1)

Predicting ESC based on Weight Change

562

(1)

ESC Behaviour of Particular Polymers

563

(15)

Polycarbonate

563

(2)

Plasticizer Migration

565

(1)

Solvents

565

(1)

Fracture-Surface Analysis

566

(2)

Illustrative Case Studies for Stress Cracking of Polycarbonate

568

(1)

Case Study 1

568

(1)

Case Study 2

569

(1)

Case Study 3

569

(1)

Case Study 4

569

(1)

Case Study 5

569

(1)

Assessing the Stress-Cracking Resistance of PC

570

(1)

Styrenics

570

(1)

SAN

571

(1)

ABS

571

(1)

HIPS

571

(1)

Polyethylenes

572

(2)

Polypropylene

574

(1)

PMMA

574

(1)

Polyurethanes

575

(1)

PET

576

(1)

Nylons

576

(1)

PVC

576

(2)

PPO

578

(1)

Investigating an ESC Failure

578

(3)

Introduction

578

(1)

Measuring Residual Stress Levels in Moulded Parts

579

(1)

Fractography

580

(1)

Analytical Methods

581

(1)

ESC Case Study

581

(6)

References

585

(2)

Residual Stresses and Weld Lines in Polymers

587

(35)

Introduction

597

Protocol for Problem-Solving Processing Defects

587

(3)

Residual Stresses and Molecular Orientation

590

(17)

Introduction

590

(1)

Residual Stresses

590

(1)

Residual Strain near Sprue

590

(1)

Wall-thickness Variations

591

(1)

Molecular Orientation

592

(1)

Frozen-In Strain in Skin Layer

592

(1)

Determination of Residual Stresses

593

(1)

Layer-Removal Procedure for Flat Mouldings

593

(1)

Residual Stresses in Pipe Walls

594

(1)

Semi-Quantitative and Non-Quantitative Methods

594

(1)

Determination of Molecular Orientation

595

(1)

Heat Reversion

595

(1)

Solvent Immersion

596

(1)

Clear Mouldings

596

(1)

Microscopy

597

(1)

Birefringence Measurements

597

(2)

Chemical Stress-Cracking Agents

599

(2)

Case studies involving stress-cracking agents

601

(3)

Control of Residual Stresses and Molecular Orientation

604

(1)

Ageing Effects

604

(1)

Effects of Residual Stresses and Molecular Orientation on Properties

605

(1)

Practical Examples of Failures related to Residual Stress and/or Molecular Orientation

606

(1)

Weldlines

607

(10)

Introduction

607

(1)

Classification of Weldlines

608

(1)

Weldlines in Polyolefins

609

(1)

Weldlines in Caps and Cylindrical Mouldings

609

(1)

Flow Weldlines in Thin-Walled Containers

609

(1)

Appearance and Location of Weldlines

610

(1)

Strength of Weldlines

611

(1)

Factors Affecting Weldline Characteristics

611

(1)

Mould Design Aspects

611

(2)

Processing Variables

613

(1)

Effect of Additives on Weldline Strength

613

(1)

Effect of Polymer Type on Weldline Strength

613

(1)

Assessing the Contribution of Weldlines to Part Failure

614

(1)

Practical Examples of Weldline-Related Failures

614

(3)

Shrinkage and Warpage

617

(5)

Introduction

617

(1)

Factors Affecting Shrinkage and Warpage

617

(1)

Determination of Shrinkage and Warpage

618

(1)

References

619

(3)

Odour, Tainting and Outgassing Problems with Polymers

622

(25)

Odour Problems in Polymers

622

(10)

Introduction

622

(2)

Origins of Odour-Causing Compounds

624

(1)

Manufacturing Processes

624

(1)

Polyethylenes

624

(1)

Polyurethanes

625

(1)

Residual Monomer

626

(1)

Processing

626

(1)

Additives

627

(1)

Initiators

627

(1)

Chain-transfer agents

627

(1)

Plasticizers

628

(1)

Pigments

629

(1)

Stabilizers

629

(1)

Lubricants

629

(1)

Slip agents

629

(1)

Nucleating agents

630

(1)

Cross linking agents

630

(1)

Blowing agents

631

(1)

Curing

631

(1)

Use of Odour Adsorbers

631

(1)

Analysis Methods

631

(1)

Taste and Off-Flavours

632

(4)

Tainting of Plastic Containers

633

(1)

PET Bottles

633

(1)

HDPE Bottles

633

(1)

Adventitious additives

634

(1)

LDPE Bottles and Pouches

634

(1)

Taste Testing

635

(1)

Analytical Analysis of Off-Flavours

635

(1)

Out-Gassing

636

(4)

Introduction

636

(1)

Common Types of Out-Gassing

637

(1)

Formaldehyde Vapours

637

(1)

Emissions from Car Interiors

637

(1)

Outgassing from Synthetic Carpets

638

(1)

Process Solvents

639

(1)

Residual Monomer

639

(1)

Analysis of Organic Vapours Emitted from Polymers

640

(1)

Volatiles in Polymers and Their Detection

640

(7)

Volatiles

640

(1)

Analysis Methods

640

(1)

GC-MS

641

(1)

Head-Space Analysis

641

(1)

Evolved-Gas Analysis

642

(1)

TG-MS

642

(1)

Thermolysis-MS

643

(1)

Sample Handling

643

(1)

Simple-Trapping Methods

644

(1)

Comparison of Trapping Materials for Volatiles

644

(1)

Advanced Techniques

645

(1)

References

645

(2)

Adhesion Problems with Polymers and Interfaces

647

(23)

Introduction

647

(2)

Case Studies

649

(11)

Polyolefins

649

(1)

Surface Contamination of Polyolefins

650

(1)

Interfacial Adhesion in Composites

651

(2)

Investigation of the Adhesion Interface in Composites

653

(1)

Topography of the Interface

653

(1)

Weak Surface Layers

654

(1)

Chemical Nature of Reinforcement Surface

654

(1)

Detecting Residual Sizing Agent

654

(1)

Determining the Presence of Coupling Agents or Surface Treatment Materials

655

(1)

Moisture Diffusion in Composites

655

(1)

Analysis of Fibre-Matrix Adhesion

655

(1)

Sealant Failure

656

(1)

Chemical Attack of Silicones

657

(1)

Hydrolytic Deterioration of Silicone Sealants

657

(2)

Modes of Sealant Failure

659

(1)

Common Classes of Polymeric Adhesives

660

(2)

Epoxies

660

(1)

Polyurethanes

660

(1)

Cyanoacrylates

661

(1)

Silicone Sealants

661

(1)

Solvent Adhesives

661

(1)

Common Causes of Adhesive Failure

662

(8)

Topography

662

(1)

Weak Surface Layers

663

(1)

Oxidative Degradation

664

(1)

Chemical Attack

665

(1)

Cure-Related Factors

665

(2)

Gap-Filling Problems

667

(1)

Thermal Mismatch

667

(1)

Water Penetration

667

(1)

Entrapped Solvent

668

(1)

Stress

668

(1)

References

668

(2)

Voids, Blisters and Surface Defects

670

(22)

Voids

670

(13)

Introduction

670

(2)

Voids in Injection-Moulded Products

672

(3)

Voids in Rotomoulded Products

675

(2)

Voids due to Volatiles

677

(2)

Voids due to Welding

679

(1)

Voids in Composites

679

(1)

Voids in Two-Part Thermosetting Polymers

680

(1)

Voids in Sintered Components

680

(1)

Voids in Cable Insulation

681

(1)

Methodology for Problem Solving

681

(2)

Blisters

683

(6)

Introduction

683

(2)

Blisters due to Vapour Permeation

685

(1)

Blisters in Polymeric Surface Coatings (Paints)

686

(2)

Blisters in Polymer Composites

688

(1)

Surface Defects

689

(3)

Surface Blemishes

689

(1)

Weldline Surface Defects

689

(1)

Lenses in Films

690

(1)

Melt Fracture

690

(1)

Pin-Holing

690

(1)

Other Surface Defects

690

(1)

References

691

(1)

Discoloration of Polymers

692

(49)

Introduction

692

(5)

Steps for Polymer Discoloration Problem Solving

693

(3)

Some Difficulties in Studying Discoloration

696

(1)

Classification of Polymer Discoloration

696

(1)

Polyolefins

697

(19)

Antioxidant Conversion Products

698

(3)

General Analysis for AO Conversion Products

701

(5)

Antioxidant-Metal Ion Interactions

706

(2)

General Analysis for AO-Metal Ion Complexes

708

(1)

Antioxidant-TiO2 Interactions

709

(2)

Antioxidant-Acid Interactions

711

(1)

Storage Yellowing

711

(1)

Fabric Discoloration

712

(1)

General Analysis for NOx Yellowing

713

(1)

Cardboard Yellowing

713

(1)

Discoloration due to Amine-Based Additives

714

(1)

Aromatic Amines

714

(1)

Hindered-Amine Light Stabilizers

715

(1)

Antistatic Agents

715

(1)

Aromatic Polymers Containing Ph--O or Ph--N Linkages

716

(5)

Polycarbonate

716

(1)

Polyurethanes

717

(1)

Poly(Phenylene Oxide)

718

(2)

Unsaturated Polyesters

720

(1)

Polysulfones

720

(1)

Aromatic Polymers containing Ph-C=O or Ph-S Linkages

721

(5)

Poly(Ethylene Terephthalate)

721

(2)

Aliphatic Polyamides (Nylons)

723

(1)

Aromatic Polyamides (Aramids)

724

(1)

Poly(Phenylene Sulfide)

725

(1)

Nitrile Polymers

726

(3)

Polyacrylonitrile

726

(1)

Poly(Styrene-co-Acrylonitrile)

727

(1)

Acrylonitrile-Butadiene-Styrene

728

(1)

Vinyl Polymers

729

(4)

Poly(Vinyl Chloride)

729

(2)

Ethylene-Vinyl Acetate Copolymers

731

(2)

Poly(Vinylidene Fluoride)

733

(1)

Miscellaneous Polymers

733

(3)

Polystyrene

733

(1)

High-Impact Polystyrene

734

(1)

Poly(Methyl Methacrylate) and Photocured Acrylates

735

(1)

Polyoxymethylene

735

(1)

Radiation Yellowing

736

(5)

References

738

(3)

Index

741

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Compositional and Failure Analysis of Polymers A Practical Approach

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Compositional and Failure Analysis of Polymers A Practical Approach

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