AND FABRICATED nalysis of Plastic and Rubber …lib3.dss.go.th/fulltext/index/668/668.41han.pdfIndex . Acid digestion of plastics chemical reagents, 541-545 closed vessels, acid digestion

nalysis of Plastic and Rubber Materials

STM SPECIFICATION AND FABRICATED

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Index

Acid digestion of plastics chemical reagents, 541-545 closed vessels, acid digestion in,

543-544 microwave acid digestion, 544-545 open-vessel acid digestion, 543

Acrylate polymers, 240--242 Acrylonitrile, 587, 588 Acrylonitrile- bu tadiene-styrene

copolymers, 253-255 decomposition temperature, 126

Acylation, gas chromatography, 382 Additive content, determination of,

thermogravimetric analysis of polymers, 121

Additives in plastics, analysis by, chromatography, differential scanning, 88-89

Aging, physical, thermogravimetric analysis of polymers, 119

Alginates, 590 Aliphatic polyesters, 462

nuclear magnetic resonance solvent, 417

Aliphatic polyethers, 462 Aliphatic polymers, 262-265 Alkyd resins, 273-275 Alkylation, gas chromatography, 382 Alumel, Curie temperature, 117

Aluminum-clad columns, high-temperature gas chromatography, 389

Amino polymers, 279 melamine-based resins, 281 urea-formaldehyde resins, 279-281

Analysis of particle size, 38 optical microscopy, 38 particle-size distribution

measurement, 38 sieving, 38

Anion separation, capillary electrophoresis, 536--537

Antimony, ash temperature, graphite furnace, 518

Anti-Stokes scattering, 293 Aromatic polyesters, 462

nuclear magnetic resonance solvent, 417

Aromatic polyethers, 262-265, 462 Arsenic, ash temperature, graphite

furnace, 518 Artificial intelligence, gas

chromatography, 398-399 Ash content, 39 Ash temperatures, with graphite

furnace, 518

I

I" I

Atomic absorption spectrophotometry, 34-35

629

630

Atomic spectroscopy, 511, 513-524 analytical techniques, 514 inorganic analyses, polymers, 511

Automatic titration, 31

Bagley correction, 51-53 Barium fluoride, optical properties of,

300 Baseline subtraction, in running

sample, differential scanning chromatography, 105-106

Benzenes, substituted, 214-217 Bismuth, ash temperature, graphite

furnace, 518 Bisphenol polyester resins, 276 Butadiene, 588 Butadiene resins, 249 Butadiene rubber, 587 Butadiene styrene, 588 Butyl phenol resin, 278

Cadmium, ash temperature, graphite furnace, 518

Cadmium telluride, optical properties of, 300

Calcium fluoride, optical properties of, 300

Calibration, differential scanning chromatography, 96-99

Calibration techniques, thermogravimetric analysis of polymers, 113-117

calcium oxalate monohydrate, measuring weight loss with temperature, 115-117

furnace calibration, 115 temperature calibration, 115 weight calibration, 113

Calorimetry, differential scanning, 79-110

additives in plastics, treatments or plastics, analysis by, 88-89

applications, 81-92 calibration, 96--99

instrument, 95-99

lnderIndex

[Calorimetry, differential scanning] Capil

characterizing sample, 106-107 Capil

coolants, 103 Ba

curling studies, 85 cal enthalpy of melting, 83-85 cor

gas, purge of, 102-103 dat

glass transition temperature, 81-82 heat history, effects of, 104-105 r

history of. 92-93 melting temperature, 83 die

oxidative stability testing, 87-88 me.

pan, selecting, sample size for me experiment, 103 me.

recrystallization Ne' temperature, upon cooling, 85-87 time. 87 Ral

reproducible experiments, tests, run 1,93-108

running sample, baseline P subtraction, 105-106 P

sample pan selection, 100-102 s·

sample preparation, 99-100 sen

sample size, 99 d scanning rates, effects of, 104 temperature-dependent crystallinity,

89-91 d test methods, 107-108 -

Capillary columns, gas chromatography, 345-351

stationary phase, 346-348 s Capillary electrophoresis, 12, 512, tl

532-540 slit

anion separation, 536-537 stes

background, 532 teel capillary electrophoresis theory, the'

533-534 the

capillary zone electrophoresis, tim

534-536 cation separation, 536 - Capil

detection, 539 instrumentation, 537-539 - Carbe

ionic separation, 539-540 Carbr

theory, 533-534 vs. ion chromatography, 539 - Carb

Capillary rheology, 21 Carra

c

631 Index

[Calorimetry, differential scanning] characterizing sample, 106-107 coolants, 103 curling studies, 85 enthalpy of melting, 83-85 gas, purge of, 102-103 glass transition temperature, 81-82 heat history, effects of, 104-105 history of, 92-93 melting temperature, 83 oxidative stability testing, 87-88 pan, selecting, sample size for

experiment, 103 recrystallization

temperature, upon cooling, 85-87 time, 87

reproducible experiments, tests, 93-108

running sample, baseline subtraction, 105-106

sample pan selection, 100-102 sample preparation, 99-100 sample size, 99 scanning rates, effects of, 104 temperature-dependent crystallinity,

89-91 test methods, 107-108

Capillary columns, gas chromatography, 345-351

stationary phase, 346-348 Capillary electrophoresis, 12, 512,

532-540 anion separation, 536-537 background, 532 capillary electrophoresis theory,

533-534 capillary zone electrophoresis,

534-536 cation separation, 536 detection, 539 instrumentation, 537-539 ionic separation, 539-540 theory, 533-534 vs. ion chromatography, 539

Capillary rheology, 21

Index

Capillary rheometers, 53-56 Capillary rheometry, 43-78

Bagley correction, 51-53 capillary rheometers, 53-56 common accessories, 75 data interpretation, 67-72

data presentation, 69-70 material characterization, 67-69 quality control, 70--72

die swell measurement, 75 melt density, 74-75 melt indexers, 56-57 melt tensile tests, 75-76 Newtonian equations, for round-

hole capillary flow, 46-48 Rabinowitch correction, 48-51 running test, 62-67

loading rheometer, 63-64 possible problems, 64-67 preparing rheometer, 62-63 sample preparation, 62

setup parameters, 57--62 determining number of shear

rate points per curve, 60--61

die length, pressure transducer selection, 60

shear range, die diameter selection, 58-59

shear rate order, 61-62 temperature, 58

slit die capillaries, 48 steady shear viscosity, 44-46 techniques, 57-67 theory, 44-53 thermal stability, 73-74 time-temperature superposition,

72-73 Capillary zone electrophoresis,

534-536 Carbon analysis, 35-36 Carbon-carbon double bonds,

211-214 Carboxymethylcellulose, 588 Carrageenan, 590

Carrier gas, gas chromatography, 361-366

gas generators, 366 gas purity, purification, 364-366

moisture traps, 365 oxygen traps, 365-366

selecting, 361-364 van Deemter curves, 362

Cation separation, capillary electrophoresis, 536

Cellulose, 288, 590 Cellulose acetate, 288-290, 587 Cellulose derivatives, 287-290

cellulose, 288 cellulose acetate, 288-290

Cellulose triacetate, 587 Cesium iodide, optical properties of,

300 Characterization of polymers, 208-216 Chemical shift, in nuclear magnetic

resonance, 408--410 Chemiluminescence-redox detector,

374 Chitosan, 590 Chlorinated polyethylene, 589 Chlorine analysis, 31-32 Chromatography. See Gas

chromatography Chromel A, temperature limits, 115 Chromium, ash temperature, graphite

furnace, 518 Closed vessels, acid digestion in,

543-544 Cobalt, ash temperature, graphite

furnace, 518 Cold trapping, gas chromatography,

356 Collagen, 590 Color measurements, 40 Conductivity, thermal, 129-154

amorphous materials, 143-145 ASTM standards, 132 chemical reaction, effect of, 149 comparative method, 135-137 composition, effect of, 147-149

632

[Conductivity, thermal] crystallinity, effect of, 146 guarded hot-plate technique, 132-133 heat flow meter, 132 heat-flow meters, 133-135 laser-flash thermal diffusivity, 132,

140-141 line-source method, 132, 137-140 pressure, effect of, 147 standards, 131 thermal contact resistance, 141-143

Configurational isomerism, nuclear magnetic resonance, 469--475

Contaminates in polymers, 545-546 Convection oven, moisture by, 37 Coolants, differential scanning

chromatography, 103 Cooling, recrystallization temperature

upon, chromatography, differential scanning, 85-87

Copper, ash temperature, graphite furnace, 518

Creep, 29-30 Cresol resin, 278 Cryofocusing technology, 394---397 Crystallinity

in polymer systems, 209-210 temperature-dependent,

chromatography, differential scanning, 89-91

Cubic zirconia, optical properties of, 300

Curie temperatures, 117 Curling studies, chromatography,

differential scanning, 85

Data interpretation, capillary rheometry, 67-72

data presentation, 69-70 material characterization, 67-69 quality control, 70-72

Degradation temperature, determination of, thermogravimetric analysis of polymers, 117-119

Index

Densitometry, 20 Density in polymer systems, 209-210 Derivatization reactions, gas

chromatography, 381-382 Detector selection, gas

chromatography, 366-375 chemiluminescence-redox detector,

374 combination detectors, 375 electrolytic conductivity detector,

373 electron-capture detector, 370-371 flame ionization detector, 369 flame photometric detector, 371 Fourier transform infrared

detectors, 373-374 inductively coupled plasma

ionization, 375 ion mobility detector, 374 isotope ratio mass spectrometry,

374---375 linear range, 367-368 makeup gas, 366 mass spectrometer, 373-374 nitrogen-phosphorous detector,

369-370 photoionization detector, 371-372 selectivity, 367 sensitivity, 367 surface ionization detector, 374 tandem PIDjFID combination

detector, 372 thermal conductivity detector, 368

Dextrans, 590 Diallyl phthalate, 587 Diamond, optical properties of, 300 Die swell measurement, capillary

rheometry, 75 Dielectric analyzer, 28 Differential photocalorimetry, 24 Differential scanning calorimetry, 24,

79-110 additives in plastics, treatments or

plastics, analysis by, 88-89 applications, 81-92

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633 Index

snsitometry, 20 msity in polymer systems, 209-210 erivatization reactions, gas

chromatography, 381-382 etector selection, gas

chromatography, 366--375 chemiluminescence-redox detector,

374 combination detectors, 375 electrolytic conductivity detector,

373 electron-capture detector, 370--371 flame ionization detector, 369 flame photometric detector, 371 Fourier transform infrared

detectors, 373-374 inductively coupled plasma

ionization, 375 ion mobility detector, 374 isotope ratio mass spectrometry,

374-375 linear range, 367-368 makeup gas, 366 mass spectrometer, 373-374 nitrogen-phosphorous detector,

369-370 photoionization detector, 371~372

selectivity, 367 sensitivity, 367 surface ionization detector, 374 tandem PIDjFID combination

detector, 372 thermal conductivity detector, 368 extrans, 590 iallyl phthalate, 587 iamond, optical properties of, 300 ie swell measurement, capillary

rheometry, 75 ielectric analyzer, 28 ifferential photocalorimetry, 24 ifferential scanning calorimetry, 24,

79-110 additives in plastics, treatments or

plastics, analysis by, 88-89 applications, 81-92

Index

[Differential scanning calorimetry] calibration, 96--99

instrument, 95-99 characterizing sample, 106--107 coolants, 103 curling studies, 85 enthalpy of melting, 83-85 gas, purge of, 102-103 glass transition temperature, 81-82 heat history, effects of, 104-105 history of, 92-93 melting temperature, 83 oxidative stability testing, 87-88 pan, selecting, sample size for

experiment, 103 recrystallization temperature, upon

cooling, 85-87 recrystallization time, 87 reproducible experiments, tests,

93-108 running sample, baseline

subtraction, 105-106 sample pan selection, 100--102 sample preparation, 99-100 sample size, 99 scanning rates, effects of, 104 temperature-dependent crystallinity,

89-91 test methods, 107-108

Diffraction particle size measurements, laser, 594-602

Diffusion measurements, nuclear magnetic resonance, 435-436, 456-457

Diffusivity, thermal, 149-151 Dipolar coupling, nuclear magnetic

resonance, 407-408 Direct flash vaporization liners, gas

chromatography, 360 Direct injection, gas chromatography,

357-358 Dynamic mechanical analysis, 26--27,

155--200 applications, 174-194 cured thermosets, 174-184

[Dynamic mechanical analysis] forced frequency analyzers,

167-169 free-resonance analyzers, 170--172 instrumentation, 172-174 PerkinElmer DMA 7e, 173 polymer melts, solutions, 184-188 Rheometric Sciences SR-5, 173 thermoplastic solids, 174-184

sub-TjdgjD transitions, 176--177 thermosets, 188-194

curing, 188-191 curing kinetics by, 191-192 Gillham-Enns diagram, 193-194 photocuring, 191

torsion vs. axial analyzers, 173

Electrochemical analysis, 32 Electrochemical methods, polymer

analysis, 512 Electrolytic conductivity detector, 373 Electron-capture detector, gas

chromatography, 370--371 Elemental analysis, 32-37

atomic absorption spectrophotometry, 34-35

carbon analysis, 35-36 energy-dispersive X-ray

fluorescence, 34 flame photometry, 35 halogen analysis, 36 hydrogen analysis, 35-36 inductively coupled plasma atomic

emission spectrometry, 33 inductively coupled plasma-mass

spectrometry, 32-33 Kjeldahl analysis, 35 nitrogen analysis, 35-36 oxygen analysis, 35-36 sulfur analysis, 35-36

Energy-dispersive X-ray fluorescence, 34

Enthalpy differential scanning

chromatography, 83-85

634

[Enthalpy] of melting, differential scanning

chromatography, 83-85 Environment, plastics and, 4--5 Epoxides, 284--286 Epoxy resins, 587 Ether polyurethanes, 462 Ethyl cellulose, 587 Ethylene copolymers, 228-229 Ethylene-propylene copolymers,

232-236 Ethylene-propylene diene monomer,

589

Fatigue, 30-31 Filler/additive content, determination

of, thermogravimetric analysis of polymers, 121

Fillers, laser light scattering, particle size measurement, 607-608

Flame ionization detector, gas chromatography, 369

Flame photometry, 35 detector, gas chromatography, 371

Flash gas chromatography, 392-394 cryofocusing technology, 7

Flow injection polymer analysis, 14--15 Flow nuclear magnetic resonance,

457-458 Flow techniques, nuclear magnetic

resonance, 415 Forced frequency analyzers, dynamic

mechanical analysis, 167-169 Formaldehyde, 588 Free-resonance analyzers, dynamic

mechanical analysis, 170-172

Gas, purge of, differential scanning chromatography, 102-103

Gas chromatography, 5, 7-11, 341-402 acylation, 382 alkylation, 382 analysis, 378-382 artificial intelligence, 398-399 capillary columns, 345-351

Index Inde

[Gas chromatography] [Gas stationary phase, 346-348 fib

carrier gas, 361-366 ga gas generators, 366 gas purity, purification, 364--366 selecting, 361-364 he. van Deemter curves, 362 hig

chemical ionization, 10-11 j

I column diameter, 348-349 hig column length selection, 349-350 column selection, 350-351 cryofocusing technology, 394--397 S

data recording, processing, 376-377 hig derivatization reactions, 381-382 hot detectability, reagents to enhance, inje

382 d detector selection, 366-375 il

chemiluminescence-redox detector, 374 Sj

combination detectors, 375 sl electrolytic conductivity detector, inje

373 electron-capture detector, 370-371 inje flame ionization detector, 369 ir flame photometric detector, 371 i~

Fourier transform infrared se detectors, 373-374 inlel

inductively coupled plasma ion ionization, 375 meg

ion mobility detector, 374 mull isotope ratio mass spectrometry,

374--375 new linear range, 367-368 over makeup gas, 366 lSI mass spectrometer, 373-374 tel nitrogen-phosphorous detector, patti

369-370 purg photoionization detector, 371-372 pyro selectivity, 367 sensitivity, 367 quali

I

surface ionization detector, 374 an tandem PID/FID combination

detector, 372 ret thermal conductivity detector, 368 quan

I

electron impact ionization, 9-10 anI

0

635 Index

las chromatography] stationary phase, 346-348

carrier gas, 361-366 gas generators, 366 gas purity, purification, 364-366 selecting, 361-364 van Deemter curves, 362

chemical ionization, 10-11 column diameter, 348-349 column length selection, 349-350 column selection, 350-351 cryofocusing technology, 394-397 data recording, processing, 376-377 derivatization reactions, 381-382 detectability, reagents to enhance,

382 detector selection, 366-375

chemiluminescence-redox detector, 374

combination detectors, 375 electrolytic conductivity detector,

373 electron-capture detector, 370-371 flame ionization detector, 369 flame photometric detector, 371 Fourier transform infrared

detectors, 373-374 inductively coupled plasma

ionization, 375 ion mobility detector, 374 isotope ratio mass spectrometry,

374-375 linear range, 367-368 makeup gas, 366 mass spectrometer, 373-374 nitrogen-phosphorous detector,

369-370 photoionization detector, 371-372 selectivity, 367 sensitivity, 367 surface ionization detector, 374 tandem PID/FID combination

detector, 372 thermal conductivity detector, 368

electron impact ionization, 9-10

Index

[Gas chromatography] film thickness selection, 349 gas purity, purification

moisture traps, 365 oxygen traps, 365-366

headscape sampling, 384-386 high-speed, 391-394

flash, 392-394 high-temperature gas

chromatography, 389-391 aluminum-clad columns, 389 stainless steel columns, 389-391

high-volume injection, 397-398 hot on-column liners, 360-361 injection techniques, 353-361

direct injection, 357-358 injector port liners, 358-361 on-column injection, 356-357 split injection, 353-354 splitless injection, 354-356

injector port liners, direct flash vaporization liners, 360

injector selection, 351-352 injector temperatures, 352 inlet discrimination, 352 septum purge, 352

inlet system, 8-9 ion source, 9 megabore injector liners, 359 multidimensional gas

chromatography, 388 new technologies in, 388-403 oven, 375-376

isothermal operation, 376 temperature programming, 376

pattern recognition, 398-399 purge-and-trap, 384 pyrolysis gas chromatography,

382-384 qualitative analysis, 380-381

ancillary techniques, identification by, 381

retention time, 380-381 quantitative analysis, 378-380

area normalization, 379

[Gas chromatography] external standard, 380 internal standard, 379 standard addition, 380

retention-time locking, 398 sample concentration, 382-388 sample introduction, 382-388 sample preparation, 377-378 solid-phase microextraction,

387-388 split injection, split ratio, 354 split injector liners, 359 splitless injection

cold trapping, 356 solvent effect, 356

splitless injector liners, 359 stationary phase

polyethylene glycols, 347 polysiloxanes, 346-347 porous-layer phase, 347-348

straight-tube liners, 360 thermal desorption, 387

Gel permeation chromatography, 12-14, 551-554

low-angle laser light-scattering photometry, 13

multi angle laser light-scattering photometry, 13

viscosity detector for, 13-14 Germanium, optical properties of, 300 Gillham-Enns diagram, 193-194 Glass transition

temperature, differential scanning chromatography, 81-82

thermoplastic solids, 177-178 Globar, temperature limits, 115 Graphite furnace atomic absorption

spectroscopy, 515-523 alternative sample introduction,

520-521 atomization, 517-518, 521-523 background, 515-517 data analysis, 518-519 detection, 518, 523 sample introduction, 517

636

[Graphite furnace atomic absorption spectroscopy]

selecting spectroscopy technique, 523-524

Gravimetric analysis, thermal, modulated, thermogravimetric analysis of polymers, 123

Halogen analysis, 36 Headscape sampling, gas

chromatography, 384-386 Heat deflection temperature, vicat

softening point, 23-24 Heat history, effects of, differential

scanning chromatography, 104-105

Helium pycnometry, 39 High-density polyethylene

decomposition temperature, 126 different forms of, 220-221

High-environment stress-crack resistance, 225-227

High-impact polystyrene, laser light scattering, particle size measurement, 606-{i07

High-osmotic-pressure chromatography, 14

High-performance liquid chromatography, polymers, additives, 570-572

High-pressure liquid chromatography, 11

High-speed gas chromatography, 5-7, 391-394

flash gas chromatography, 6-7, 392--394

using standard instrument, 6 High-temperature gas

chromatography, 389-391 aluminum-clad columns, 389 stainless steel columns, 389-391

High-volume injection, gas chromatography, 397-398

Hisat-50, Curie temperature, 117

Index Index

[Infrare: chromatography, 360-361 phenc

Hyaluronic acid, 590 phenc Hydrochloric, physical properties of, pheny

541 poly' Hydrofluoric, physical properties of, 2

541 pol Hydrogen analysis, 35-36

Hot on-column liners, gas

polya polya

Identification, polymers, 208-216 polya Inductively coupled plasma polyb

atomic emission spectrometry, 33 polyc ionization, 375 polye mass spectrometry, 32-33 alk

Infrared analysis of polymers, 201-340 pol aliphatic polymers, 262-265 amino polymers, 279 pol

melamine- based resins, 281 • urea-formaldehyde resins, uns

279-281 polye anti-Stokes scattering, 293 polye aromatic polyethers, 262-265 eth bisphenol polyester resins, 276 ger butadiene resins, 249 hig butyl phenol resin, 278 cellulose derivatives, 287-290 hig

cellulose, 288 • cellulose acetate, 288-290 lOr

characterization of polymers, I lin 208-216

cresol resin, 278 lor crystallinity, in polymer systems, ter

209-210 poly! density in polymer systems, 209-210 polyi epoxides, 284-286 polyi experimental procedures, 290-304 gases, 299 polyi identification, polymers, 208-216 polyi instrumentation, 295-298 poly,

I Iliquids, 299-302 etl

microstructures, correlation, functional groups, 211-217 pc

carbon-carbon double bonds, pc 211-214 poly

substituted benzenes, 214--217 polyI

637 Index

on-column liners, gas chromatography, 360-361

uronic acid, 590 .ochloric, physical properties of,

541 .ofluoric, physical properties of,

541 rogen analysis, 35-36

tification, polymers, 208-216 ctively coupled plasma rmic emission spectrometry, 33 iization, 375 iSS spectrometry, 32-33 .red analysis of polymers, 201-340 phatic polymers, 262-265 iino polymers, 279 melamine-based resins, 281 urea-formaldehyde resins,

279-281 ti-Stokes scattering, 293 omatic polyethers, 262-265 .phenol polyester resins, 276 .tadiene resins, 249 .tylphenol resin, 278 llulose derivatives, 287-290 cellulose, 288 cellulose acetate, 288-290 aracterization of polymers,

208-216 esol resin, 278 ystallinity, in polymer systems,

209-210 nsity in polymer systems, 209-210 oxides, 284-286 perimental procedures, 290-304 ses,299 entification, polymers, 208-216 strumentation, 295-298 uids, 299-302 .crostructures, correlation,

functional groups, 211-217 carbon-carbon double bonds,

211-214 substituted benzenes, 214-217

Index

[Infrared analysis of polymers] phenol resin, 278 phenolic resins, 277-279 phenyl-phenol resin, 278 poly "halogenated" ethylenes,

242-248 polymers of, 247

polyamides, 256-261 polyamidimide, 267-268 polyarylsulfones, 265-266 polybutadiene, 248-249 polycarbonates, 261-262 polyesters, 270-276

alkyd resins, 273-275 polybutylene terephthalate,

270-273 polyethylene terephthalate,

270-273 unsaturated polyesters, 275-276

polyethersulfones, 265-266 polyethylene

ethylene copolymers, 228-229 general characterization, 219-220 high-density polyethylene,

different forms of, 220-221 high-environment stress-crack

resistance, 225-227 ionomers, 228-229 linear low-density polyethylene,

different forms of, 221-224 long-chain branching, 225 terminal methyl content, 225

polyethylene oxide, 262-263 polyimide, 267-268 polymer chains, orientation of,

210-211 polymer characterization, 217-290 polymer identification, 203-207 polyolefins, 217-236

ethylene-propylene copolymers, 232-236

polyethylene, 217-229 polypropylene, 230-232

polyoxymethylene, 262-263 polyphenylene oxide, 264-265

[Infrared analysis of polymers] polyphenylene sulfide, 266-267 polypropylene oxide, 262-263 polysiloxanes, 281-284 polystyrene, 249-256

acrylonitrile-butadiene-styrene copolymers, 253-255

styrene-butadiene copolymers, 251-252

polysulfones, 265-266 polytetrafluoroethylene, 247 polyurethanes, 269-270 polyvinyl chloride, 242-243 Raman effect, 293 Rayleigh scattering, 293 resolcinol resin, 278 sample handling methods, 298-304 silicone-based polymers, 281-284 solids, 302-304 spectroscopy, general principles,

290-295 Stokes scattering, 293 substituted butadiene, polymers of,

248-249 vapors, 299 vinyl chloride, polymers of, 242-248 vinyl chloride-vinyl acetate

copolymers, 243-245 vinyl polymers with ester groups,

236-242 acrylate polymers, 240-242 methacrylate, 240-242 polyvinyl acetate, 236-239 polyvinyl alcohol, 239-240 vinyl acetate-ethylene copolymer,

236-239 vinylidene chloride copolymers,

245-246 window materials, optical properties

of, 300 xylenol resin, 278

Infrared spectroscopy, 15-16 Injection techniques, gas

chromatography, 353-361 direct injection, 357-358

&38

[Injection techniques, gas chromatography]

injector port liners, 358-361 direct flash vaporization liners,

360 hot on-column liners, 360-361 megabore injector liners, 359 split injector liners, 359 splitless injector liners, 359 straight-tube liners, 360

on-column injection, 356-357 split injection, 353-354

split ratio, 354 splitless injection, 354--356

cold trapping, 356 solvent effect, 356

Injector port liners, gas chromatography, 358-361

direct flash vaporization liners, 360 hot on-column liners, 360-361 megabore injector liners, 359 split injector liners, 359 split less injector liners, 359 straight-tube liners, 360

Injector selection, gas chromatography, 351-352

injector temperatures, 352 inlet discrimination, 352 septum purge, 352

Injector temperatures, gas chromatography, 352

Inlet discrimination, gas chromatography, 352

Inorganic analyses, polymers, 511-548 acid digestion of plastics

chemical reagents, 541-545 closed vessels, acid digestion in,

543-544 microwave acid digestion,

544--545 open-vessel acid digestion, 543

ash temperatures, with graphite furnace, 518

atomic spectroscopy, 511, 513-524 analytical techniques, 514

Index Index

[Inorganic analyses, polymers] Ion cl capillary electrophoresis, 512, bac

532-540 dete anion separation, 536-537 inot background, 532 ion-capillary zone electrophoresis, sele

534--536 Ionm cation separation, 536 Ionic: detection, 539 capi instrumentation, 537-539 ion ionic separation, 539-540 over theory, 533-534 tech vs. ion chromatography, 539 Ionorr

contaminates in polymers, 545-546 Iron electrochemical methods, 512 ash graphite furnace atomic absorption

spectroscopy, 515-523 Cur alternative sample introduction, Isopre

520-521 IsotopI atomization, 517-518, 521-523 background, 515-517 data analysis, 518-519 Japan detection, 518, 523 • sample introduction, 517 selecting spectroscopy technique, Kanth

523-524 Kanth ion chromatography, 512 Karl I

background, 524--526 Kineti detection methods, 528-532 ion-exchange theory, 526-527 Kjelda selectivity, 527-528

I •

ionic separation, 524--540 Large ion chromatography, 524--532 • overview, 524 Laser•techniques, 524

neutron activation analysis, 512 app sample preparation, inorganic carr

analysis, 540-545 diff! introduction, 540 sample digestion, 540-545 d:

X-ray methods, 512 fillei International Organization for higl

Standardization, liquid larg

I

chromatography standards, med 583-584

I

Index

ganic analyses, polymers] iillary electrophoresis, 512,

532-540 mion separation, 536--537 oackground, 532 iapillary zone electrophoresis,

534-536 .ation separation, 536 letection, 539 nstrumentation, 537-539 onic separation, 539-540 heory, 533-534 'so ion chromatography, 539 itaminates in polymers, 545-546 :trochemical methods, 512 phite furnace atomic absorption

spectroscopy, 515-523 Iternative sample introduction,

520-521 tomization, 517-518, 521-523 ackground, 515-517 ata analysis, 518-519 etection, 518, 523 smple introduction, 517 sleeting spectroscopy technique,

523-524 chromatography, 512 ackground, 524-526 etection methods, 528-532 In-exchange theory, 526--527 :Iectivity, 527-528 c separation, 524-540 n chromatography, 524-532 zerview, 524 chniques, 524 ron activation analysis, 512 pie preparation, inorganic analysis, 540-545 troduction, 540 mple digestion, 540-545 .ymethods, 512 itional Organization for Standardization, liquid chromatography standards, 583-584

Index

Ion chromatography, 12, 512, 524-532 background, 524-526 detection methods, 528-532 inorganic analyses, polymers, 512 ion-exchange theory, 526--527 selectivity, 527-528

Ion mobility detector, 374 Ionic separation, 524-540

capillary electrophoresis, 532-540 ion chromatography, 524-532 overview, 524 techniques, 524

Ionomers, 228~229

Iron ash temperature, graphite furnace,

518 Curie temperature, 117

Isoprene, 587 Isotope ratio mass spectrometry,

374-375

Japan Industrial Standards, liquid chromatography standards, 584

Kanthal, temperature limits, 115 Kanthal super, temperature limits, 115 Karl Fischer titration, 36--37 Kinetics, reverse, thermogravimetric

analysis of polymers, 120-121 Kjeldahl analysis, 35

Large particle size, laser light scattering, 603

Laser light scattering, particle size measurement, 593-610

applications, 602-609 correlation of techniques, 604-606 diffraction particle size

measurements, 594-602 dynamic light scattering, 597-602

fillers, 607-608 high-impact polystyrene, 606--607 large particle size applications, 603 medium particle size applications,

606--607, 607-608

639

[Laser light scattering, particle size measurement]

polymer slurries, 608-609 small particle size applications,

608-609 Lead, ash temperature, graphite

furnace, 518 Lignin sulfonate, 590 Linear low-density polyethylene, forms

of, 221-224 Liquid chromatography, 11, 549-592

chemical structure, 550-551 chromatography results, 572-583

compositional determination, 580-581

design, 572-578 high-temperature soluble

polymers, 581-583 structural determination, 578-580

column conventions, 563-566 composition, 550-551 data reduction, 569-570 detection options, 568-569 elevated temperature organic soluble

polymers, 589 gel permeation chromatography,

551-554 manufacturers, 591

high-performance liquid chromatography, 570-572, 591

international standards, 583-584 molecular-weight distribution,

polymers, 550 molecular-weight values, 554-556 national standards, 583-584 organic solvents for GPC, 586 room temperature organic soluble

polymers, 587-588 sample handling, 567-568 standards, 583~584

ASTM methods, 583 DIN method, 583 International Organization for

Standardization, 583-584 Japan Industrial Standards, 584

640

[Liquid chromatography] structure-property correlations,

556-558 system configuration, 558-563 water-soluble polymers, with

methacrylate gel columns, solvent selection, 590

Long-chain branching, 225 Low-density polyethylene

decomposition temperature, 126 linear, forms of, 221-224

Lysozyme, 590

Manganese, ash temperature, graphite furnace, 518

Manufacturing, plastics and, 4 Mass spectrometer, 373-374 Mechanical testing, 28-31

creep, 29-30 fatigue, 30-31 impact, 31 modulus, stress-strain behavior,

28-29 Medium particle size, laser light

scattering, 606-607 Megabore injector liners, gas

chromatography, 359 Melamine, 588 Melamine-based resins, 281 Melt density, capillary rheometry, 74-75 Melt indexers, 56-57 Melt tensile tests, capillary rheometry,

75~76

Melt viscosity/rheology measurements, 20-23

capillary rheology, 21 cone-and-plate rheology, 21-22 extensional viscosity, 22-23 melt flow index, 20-21 slit-die rheology, 21

Melting temperature, differential scanning chromatography, 83

Mercury, ash temperature, graphite furnace, 518

Methacrylate, 240-242

Index

Methylmethacrylate, 587 Microstructures, correlation,

functional groups, 211-217 carbon-carbon double bonds, 211-214 substituted benzenes, 214-217

Microwave acid digestion, 544-545 Microwave analysis, moisture by, 37 Modulated thermal gravimetric

analysis, thermogravimetric analysis of polymers, 123

Modulus, stress-strain behavior, 28-29 Moisture analysis, 36-37

convection oven, 37 Karl Fischer titration, 36-37 microwave analysis, 37 thermogravimetric analysis of

polymers, 119-120 Molecular modeling, 41 Molybdenum, temperature limits, 115 Multiangle laser light-scattering

photometry, 13 Multicomponent polymer systems,

nuclear magnetic resonance, 495-500

additives, 500 blends, 495--498 composites, 498-500

Multidimensional gas chromatography, 388

Multidimensional nuclear magnetic resonance, 433--435, 454

N-acetylglucosamine, 590 National Institute of Standarda,

thermal conductivity, 131 Near-infrared spectrophotometry, 17 Neutron activation analysis, 512 Newtonian equations, for round-hole

capillary flow, 46--48 Nichrome, temperature limits, 115 Nickel

ash temperature, graphite furnace, 518

Curie temperature, 117 Nitric, physical properties of, 541

I lnde

Nitr Nitr

I Nuc ac

I b, bi

I cl d, di

• di

I ec ex fl( III

m

• m

I 0'

pl

• pl

• pi

Index

thylmethacrylate, 587 zostructures, correlation,

functional groups, 211-217 arbon-carbon double bonds, 211-214 ubstituted benzenes, 214-217 crowave acid digestion, 544-545 crowave analysis, moisture by, 37 dulated thermal gravimetric

analysis, thermogravimetric analysis of polymers, 123

idulus, stress-strain behavior, 28-29 iisture analysis, 36-37 :onvection oven, 37 (ad Fischer titration, 36-37 nicrowave analysis, 37 herrnogravimetric analysis of

polymers, 119-120 olecularmodeling, 41 rlybdenum, temperature limits, 115 rltiangle laser light-scattering

photometry, 13 ulticomponent polymer systems,

nuclear magnetic resonance, 495-500

additives, 500 blends, 495-498 composites, 498-500 rltidimensional gas

chromatography, 388 rltidimensional nuclear magnetic

resonance, 433-435, 454

acetylglucosamine, 590 .tional Institute of Standarda,

thermal conductivity, 131 ar-infrared spectrophotometry, 17 utron activation analysis, 512 wtonian equations, for round-hole

capillary flow, 46-48 chrome, temperature limits, 115 ckel ish temperature, graphite furnace,

2urie temperature, 117 tric, physical properties of, 541

Index

Nitrogen analysis, 35-36 Nitrogen-phosphorous detector, gas

chromatography, 369-370 Nuclear magnetic resonance, 403-510

advanced spectral interpretation, 449-458

diffusion measurements, 456-457 flow nuclear magnetic resonance,

457-458 imaging, 456-457 multidimensional nuclear

magnetic resonance, 454 relaxation measurements, 449-450 solid-state nuclear magnetic

resonance, 451-454 spectral editing, 454

basic spectral interpretation, 439-440 bulk physical properties, 485-490

morphology, 485-489 orientation, 489-490

chemical shift, 408-410 data processing, 436-438 diffusion measurements, imaging,

435-436 dipolar and quadrupolar coupling,

407-408 equipment, 412-458 experiments, 418-426, 426-436 flow techniques, 436 instrumentation, 412-414 multicomponent polymer systems,

495-500 additives, 500 blends, 495-498 composites, 498-500

multidimensional nuclear magnetic resonance, 433-435

overview, 404-411 polymer systems, applications to,

458-500 polymer-chain dynamics, 490-495

solids, 493-495 solutions, 490-493

polymer-chain structure, 460-484 branching, 467-468

641

[Nuclear magnetic resonance] configurational isomerism,

469-475 copolymer structure, 474-483 degradation mechanisms, 483-484 end groups, 468-469 material identification, 461-467

polymerization reactions, 459-460 catalysis, 459 mechanisms, 459-460

pulse nuclear magnetic resonance, 418-421

quantitation, 425-426 single-pulse experiment, 421-423,

423-425 relaxation measurements, 427-430 sample preparation, 415-418 scalar coupling, 410-411 solid-state nuclear magnetic

resonance, 430-431 solvents for polymer types, 417 special purpose instrumentation,

414-415 diffusion measurements and

imaging, 415 flow techniques, 415 solids, 414-415

spectral editing, 432-433 Zeeman interaction, 404-407

Nuclear magnetic resonance spectrometry, 16-17

Nylon 6, decomposition temperature, 126

On-column injection, gas chromatography, 356-357

Open-vessel acid digestion, 543 Optical microscopy, 38 Oven, gas chromatography, 375-376

isothermal operation, 376 temperature programming, 376

Oxidative stability testing, chromatography, differential scanning, 87-88

Oxygen analysis, 35--36

518

642

Pan selection, differential scanning calorimetry, 100-102

Particle size measurement, laser light scattering, 593-610

applications, 602-609 correlation of techniques, 604-606 large particle size applications, 603 laser diffraction particle size

measurements, 594-602 dynamic light scattering, 597-602

medium particle size applications, 606-607, 607-608

small particle size applications, 608-609

Particle-size distribution measurement, 38

Peptides, 590 Perchloric, physical properties of, 541 Perkalloy, Curie temperature, 117 Phenol resin, 278 Phenolic resins, 277-279, 587 Phenyl-phenol resin, 278 Photocuring, dynamic mechanical

analysis, 191 Photoionization detector, gas

chromatography, 371-372 Physical aging, thermogravimetric

analysis of polymers, 119 Platinum, temperature limits, 115 Poly "halogenated" ethylenes, 242-248

polymers of, 247 Poly methyl methacrylate,

decomposition temperature, 126 Poly-4-methyl pentene, 589 Polyacetals, 589 Polyacrylamide, 462, 590

nuclear magnetic resonance solvent, 417

Polyacrylates, 462 nuclear magnetic resonance solvent,

417 Polyacrylic acid, 590 Polyacrylonitrile, 462, 588 Polyaginic acid, 590 Polyamide-imide, 589

Index

Polyamides, 256-261, 462 nuclear magnetic resonance solvent,

417 Polyamidimide, 267-268 Polyarcrylonitriles, nuclear magnetic

resonance solvent, 417 Polyarylsulfones, 265-266 Polybutadiene, 248-249, 587, 588 Polybutylene terephthalate, 270-273,

588 decomposition temperature, 126

Polycarbonate, 261-262, 588 decomposition temperature, 126

Polychloroprene, 587 Polydienes, 462

nuclear magnetic resonance solvent, 417

Polydimethylsiloxane, 587 Polyepiamine, 590 Polyester alkyd resins, 587 Polyesters, 270-276

alkyd resins, 273-275 polybutylene terephthalate, 270-273 polyethylene terephthalate, 270-273 unsaturated polyesters, 275-276

Polyether sulfone, 589 Polyetheretherketone, 589

decomposition temperature, 126 Polyether-imide, 589 Polyetherketone, 589 Polyethers, nuclear magnetic resonance

solvent, 417 Polyethersulfones, 265-266 Polyethylene, 217-229, 589

ethylene copolymers, 228-229 general characterization, 219-220 high-density polyethylene, different

forms of, 220-221 high-environment stress-crack

resistance, 225-227 ionomers, 228-229 linear low-density polyethylene,

different forms of, 221-224 long-chain branching, 225 terminal methyl content, 225

In~

Po Po Po

Po Po Po Po Po Po Po Po Po Po

p(

Index

nnides, 256-261,462 clear magnetic resonance solvent,

417 imidimide, 267-268 ircrylonitriles, nuclear magnetic

resonance solvent, 417 irylsulfones, 265-266 nitadiene, 248-249, 587, 588 iutylene terephthalate, 270--273,

588 composition temperature, 126 arbonate, 261-262, 588 :omposition temperature, 126 :hloroprene, 587 Iienes, 462 clear magnetic resonance solvent,

417 limethylsiloxane, 587 piamine, 590 ster alkyd resins, 587 sters, 270--276 yd resins, 273-275 ybutylene terephthalate, 270--273 yethylene terephthalate, 270--273 iaturated polyesters, 275-276 ther sulfone, 589 theretherketone, 589 omposition temperature, 126 ther-imide, 589 therketone, 589 thers, nuclear magnetic resonance solvent, 417

thersulfones, 265-266 thylene, 217-229, 589 ylene copolymers, 228-229 eral characterization, 219-220 i-density polyethylene, different forms of, 220--221

i-environment stress-crack resistance, 225-227

rmers, 228-229 ar low-density polyethylene, different forms of, 221-224 ~-chain branching, 225 iinal methyl content, 225

Index

Polyethylene glycol, 347, 590 Polyethylene oxide, 262-263, 590 Polyethylene terephthalate, 270--273,

588 Polyethylene/ethyl acrylate, 589 Polyethyleneimine, 590 Polyethylene/rnethacrylic acid, 589 Polyethylene/vinyl acetate, 589 Polyglycolic acid, 587 Polyimide, 267-268, 589 Polyisobutylene, 587 Polyisoprene, 587 Polylysine, 590 Polymer

calibration techniques calcium oxalate monohydrate,

measuring weight loss with temperature, 115-117

furnace calibration, 115 temperature calibration, 115 weight calibration, 113

chains, orientation of, 210--211 characterization, 217-290 identification, 203-207 infrared, Raman analysis of,

201-340 thermogravimetric analysis,

111-128 aging, physical, 119 applications, 117-123 calibration techniques, 113-117 degradation temperature,

determination of, 117-119 filler/additive content,

determination of, 121 modulated thermal gravimetric

analysis, 123 moisture determination, 119-120 operation principles, 111-113 reverse kinetics, 120--121 types of plastics in one sample,

determination of, 121-122 Polymer slurries, laser light scattering,

particle size measurement, 608-609

643

Polymer solution properties, 17-20 densitometry, 20 refractometry, 20 solution viscometry, 17-20

absolute viscosity, 18 automatic relative viscometers,

18-19 falling-ball viscometers, 19-20 relative viscosity, 18 rotational viscometers, 19

Polymer systems, applications to, 458-500

Polymer-chain dynamics elastomers, 490-493 melts, 490-493 nuclear magnetic resonance,

490-495 solids, 493-495 solutions, 490-493

Polymer-chain structure, 460-484 branching, 467-468 composition, 474-483 configurational isomerism, 469-475 copolymer structure, 474-483 cross-linking, 467-468 degradation mechanisms, 483-484 end groups, 468-469 material identification, 461-467 sequence distribution, 474-483

Polymerization reactions, nuclear magnetic resonance, 459-460

catalysis, 459 mechanisms. 459-460

Polymethacrylates, 462 nuclear magnetic resonance solvent,

417 Polymethylmethacrylate, 587 Poly(n-methyl-2-vinyl pyridinium)I

salt, 590 Polyolefins, 217-236, 462

ethylene-propylene copolymers, 232-236

polyethylene, 217-229 ethylene copolymers, 228-229 general characterization, 219-220

644

[Polyolefins] high-density polyethylene,

different forms of, 220-221 high-environment stress-crack

resistance, 225-227 ionomers, 228-229 linear low-density polyethylene,

different forms of, 221-224 long-chain branching, 225 terminal methyl content, 225

polypropylene, 230-232 Polyolfefins, nuclear magnetic

resonance solvent, 417 Polyoxymethylene, 262-263 Polyphenylene oxide, 264--265, 589

decomposition temperature, 126 Polyphenylene sulfide, 266-267

decomposition temperature, 126 Polyphosphazenes, nuclear magnetic

resonance solvent, 417 Polypropylene, 230-232, 589

decomposition temperature, 126 Polypropylene oxide, 262-263 Polypropyleneglycol, 587 Polysaccharides, 590 Polysiloxanes, 281-284, 346-347, 462

nuclear magnetic resonance solvent, 417

Polystyrene, 249-256, 587, 588 acrylonitrile-butadiene-styrene

copolymers, 253-255 decomposition temperature, 126 styrene-butadiene copolymers,

251-252 Polystyrene sulfonate, 590 Polystyrene/acrylonitrile, 587 Polystyrenes, 462

nuclear magnetic resonance solvent, 417

Polysulfone, 265-266, 587 decomposition temperature, 126 nuclear magnetic resonance solvent,

417 Polytetrafluoroethylene, 247

decomposition temperature, 126

Index

Polyurethane, 269-270, 587, 588 Polyvinyl acetate, 236-239 Polyvinyl alcohol, 239-240, 590 Polyvinyl chloride, 242-243

decomposition temperature, 126 Poly(vinyl esters), 462

nuclear magnetic resonance solvent, 417

Poly(vinyl ethers), 462 nuclear magnetic resonance solvent,

417 Poly(vinyl halides), 462

nuclear magnetic resonance solvent, 417

Poly(vinyl ketones), 462 nuclear magnetic resonance solvent,

417 Poly(vinyl pyridines), 462

nuclear magnetic resonance solvent, 417

Polyvinyl pyrrolidone, 590 Polyvinylacetate, 587 Polyvinylamine, 590 Polyvinylbutyral, 587 Polyvinylchloride, 587 Polyvinylcloride, 587 Polyvinylformal, 587 Polyvinylidene fluoride, 589

decomposition temperature, 126 Poly(vinylidene halides), 462

nuclear magnetic resonance solvent, 417

Polyvinylidenechloride, 587 Potassium bromide, optical properties

of, 300 Product design, plastics and, 3--4 Propylene diene monomer, 589 Pullulans, 590 Pulse nuclear magnetic resonance,

418--421 quantitation, 425--426 single-pulse experiment, 421--423,

423--425 Purge-and-trap, gas chromatography,

384

Inl

Py

Qt

Qt

Qt

R, R,

Index

yurethane, 269-270, 587, 588 yvinyl acetate, 236-239 yvinyl alcohol, 239-240, 590 yvinyl chloride, 242-243 ecomposition temperature, 126 y(vinyl esters), 462 uclear magnetic resonance solvent,

417 ~(vinyl ethers), 462 uclear magnetic resonance solvent,

417 ~(vinyl halides), 462 uclear magnetic resonance solvent,

417 ~(vinyl ketones), 462 uclear magnetic resonance solvent,

417 /(vinyl pyridines), 462 uclear magnetic resonance solvent,

417 zvinyl pyrrolidone, 590 rvinylacetate, 587 zvinylamine, 590 rvinylbutyral, 587 rvinylchloride, 587 rvinylcloride, 587 rvinylformal, 587 rvinylidene fluoride, 589 xomposition temperature, 126 '(vinylidene halides), 462 iclear magnetic resonance solvent,

417 vinylidenechloride, 587 issium bromide, optical properties

of,300 luct design, plastics and, 3--4 iylene diene monomer, 589 Idans,590 e nuclear magnetic resonance,

418--421 iantitation, 425--426 igle-pulse experiment, 421--423,

423--425 :e-and-trap, gas chromatography,

384

Index

Pyrolysis gas chromatography, 382-384

Quadrupolar coupling, nuclear magnetic resonance, 407--408

Qualitative analysis, gas chromatography, 380-381

ancillary techniques, identification by, 381

retention time, 380-381 Quantitative analysis, gas

chromatography, 378-380 area normalization, 379 external standard, 380 internal standard, 379 standard addition, 380

Rabinowitch correction, 48-51 Raman analysis of polymers, 201-340

aliphatic polyethers, 262-265 amino polymers, 279

melamine-based resins, 281 urea-formaldehyde resins, 279-281

aromatic polyethers, 262-265 bisphenol polyester resins, 276 cellulose derivatives, 287-290

cellulose, 288 cellulose acetate, 288-290

epoxides, 284--286 experimental procedures, 290-304

anti-Stokes scattering, 293 gases, 299 instrumentation, 295-298 liquids, 299-302 Raman effect, 293 Raman spectroscopy, 290-295 Rayleigh scattering, 293 sample handling methods,

298-304 solids, 302-304 Stokes scattering, 293 vapors, 299

phenolic resins, 277-279 poly "halogenated" ethylenes,

242-248

645

[Raman analysis of polymers] polyamides, 256-261 polyamidimide, 267-268 polycarbonates, 261-262 polyesters, 270-276

alkyd resins, 273-275 polybutylene terephthalate,

270-273 polyethylene terephthalate,

270-273 unsaturated polyesters, 275-276

polyethylene oxide, 262-263 polyimide, 267-268 polymer characterization, 217-290 polyoxymethylene, 262-263 polyphenylene oxide, 264--265 polyvinyl chloride, 242-243 vinyl chloride, polymers of, 242-248 vinyl chloride-vinyl acetate

copolymers, 243-245 vinylidene chloride copolymers,

245-246 Raman effect, 293 Rayleigh scattering, 293 Recrystallization

temperature, upon cooling, chromatography, differential scanning, 85-87

time, chromatography, differential scanning, 87

Refractometry, 20 Relaxation measurements, nuclear

magnetic resonance, 427--430, 449--450

Resolcinol resin, 278 Retention-time locking, gas

chromatography, 398 Reverse kinetics, thermogravimetric

analysis of polymers, 120-121 Rheology measurements, 20-23

capillary rheology, 21 cone-and-plate rheology, 21-22 extensional viscosity, 22-23 melt flow index, 20-21 slit-die rheology, 21

646

Rheometry, capillary, 43-78 Bagley correction, 51-53 capillary rheometers, 53-56 common accessories, 75 data interpretation, 67-72

data presentation, 69-70 material characterization,

67-69 quality control, 70--72

die swell measurement, 75 melt density, 74-75 melt indexers, 56--57 melt tensile tests, 75-76 Newtonian equations, for

round-hole capillary flow, 46-48

Rabinowitch correction, 48-51 running test, 62-67

loading rheometer, 63-64 possible problems, 64-67 preparing rheometer, 62-63 sample preparation, 62

setup parameters, 57-62 determining number of shear

rate points per curve, 60--61

die length, pressure transducer selection, 60

shear range, die diameter selection, 58-59

shear rate order, 61-62 temperature, 58

slit die capillaries, 48 steady shear viscosity, 44-46 techniques, 57-67 theory, 44-53 thermal stability, 73-74 time-temperature superposition,

72-73 Rhodium, temperature limits, 115 Rosin acids, 587 Round-hole capillary flow, Newtonian

equations, 46-48 Rubbery plateau, thermoplastic solids,

179-181

Index

Sample preparation differential scanning

chromatography, 99--100 inorganic analysis, 540--545

introduction, 540 sample digestion, 540--545 wet ashing, 540--545

Sapphire, optical properties of, 300 Scalar coupling, nuclear magnetic

resonance, 410-411 Scanning calorimetry, differential,

79-110 additives in plastics, treatments or

plastics, analysis by, 88-89 applications, 81-92 calibra tion, 96--99

instrument, 95-99 characterizing sample, 106--107 coolants, 103 curling studies, 85 enthalpy of melting, 83-85 gas, purge of, 102-103 glass transition temperature,

81-82 heat history, effects of, 104-105 history of, 92-93 melting temperature, 83 oxidative stability testing, 87-88 pan, selecting, sample size for

experiment, 103 recrystallization

temperature, upon cooling, 85-87

time, 87 reproducible experiments, tests,

93-108 running sample, baseline

subtraction, 105-106 sample pan selection, 100--102 sample preparation, 99-100 sample size, 99 scanning rates, effects of, 104 temperature-dependent crystallinity,

89-91 test methods, 107-108

In

Sc

Sc

Se

Index

nple preparation lifferential scanning

chromatography, 99-100 norganic analysis, 540-545

introduction, 540 sample digestion, 540-545 wet ashing, 540-545

iphire, optical properties of, 300 lar coupling, nuclear magnetic

resonance, 410-411 nning calorimetry, differential,

79-110 dditives in plastics, treatments or

plastics, analysis by, 88-89 pplications, 81-92 alibration, 96-99 instrument, 95-99

haracterizing sample, 106-107 oolants, 103 urling studies, 85 nthalpy of melting, 83-85 as, purge of, 102-103 lass transition temperature,

81-82 eat history, effects of, 104-105 istory of, 92-93 ielting temperature, 83 xidative stability testing, 87-88 an, selecting, sample size for

experiment, 103 ecrystallization temperature, upon cooling,

85-87 time, 87

eproducible experiments, tests, 93-108

unning sample, baseline subtraction, 105-106

ample pan selection, 100-102 ample preparation, 99-100 ample size, 99 canning rates, effects of, 104 smperature-dependent crystallinity,

89-91 st methods, 107-108

Index

Scanning electron microscopyjenergy dispersive X-ray fluorescence spectrometry, 39

Scanning rates, effects of, differential scanning chromatography, 104

Separation methods, 5-14 capillary electrophoresis, 12 flash gas chromatography,

cryofocusing technology, 7 gas chromatography, 5, 7-11

chemical ionization, 10-11 electron impact ionization, 9-10 inlet system, 8-9 ion source, 9

gel permeation chromatography, 12-14

high-osmotic-pressure chromatography, 14

high-pressure liquid chromatography, 11

high-speed gas chromatography, 5-7 flash gas chromatography, 6-7 using standard instrument, 6

ion chromatography, 12 liquid chromatography, 11 mass spectrometry, 7-11 size-exclusion chromatography (gel

permeation chromatography), 12-14

low-angle laser light-scattering photometry, 13

multiangle laser light-scattering photometry, 13

viscosity detector for, 13-14 thin-layer chromatography, 12

Septum purge, gas chromatography, 352

Setup parameters, capillary rheometry, 57-62

determining number of shear rate points per curve, 60-61

die length, pressure transducer selection, 60

shear range, die diameter selection, 58-59

647

[Setup parameters, capillary rheometry] shear rate order, 61-62 temperature, 58

Sieving, 38 Silicon, optical properties of, 300 Silicone-based polymers, 281-284 Silver bromide, optical properties of,

300 Size, sample, differential scanning

chromatography, 99 Size-exclusion chromatography (gel

permeation chromatography), 12-14

low-angle laser light-scattering photometry, 13

multiangle laser light-scattering photometry, 13

viscosity detector for, 13-14 Slit die capillaries, 48 Slurries, polymer, laser light scattering,

particle size measurement, 608-609

Small particle size, laser light scattering, 608-609

Sodium chloride, optical properties of, 300

Solid-phase microextraction, gas chromatography, 387-388

Solid-state nuclear magnetic resonance, 430-431, 451--454

Solution viscometry, 17-20 absolute viscosity, 18 automatic relative viscometers,

18-19 falling-ball viscometers, 19-20 relative viscosity, 18 rotational viscometers, 19

Solvents, for polymer types, nuclear magnetic resonance, 417

Spectral editing, nuclear magnetic resonance, 432--433, 454

Spectroscopic analysis, 15-17 infrared spectroscopy, 15-16 near-infrared spectrophotometry,

17

648

[Spectroscopic analysis] nuclear magnetic resonance

spectrometry, 16-17 ultra violet-visible

spectrophotometry, 17 Spectroscopy, general principles,

290--295 Split injector liners, gas

chromatography, 359 Splitless injection, gas

chromatography, cold trapping, 356

Splitless injector liners, gas chromatography, 359

Stainless steel columns, high­temperature gas chromatography, 389~391

Stationary phase, capillary columns, gas chromatography, 346-348

Steady shear viscosity, capillary rheometry, 44-46

Stokes scattering, 293 Straight-tube liners, gas

chromatography, 360 Stress-crack resistance, high-

environment, polymer, 225-227 Styrene, 587 Styrene-butadiene copolymers, 251-252 Substituted benzenes, 214-217 Substituted butadiene, polymers of,

248-249 Sulfur analysis, 35-36 Sulfuric, physical properties of, 541 Surface ionization detector, 374

Tantalum, temperature limits, 115 Temperature-dependent crystallinity,

chromatography, differential scanning, 89-91

Terminal methyl content, polymer, 225 Test, capillary rheometry, 62-67

loading rheometer, 63-64 possible problems, 64-67 preparing rheometer, 62-63 sample preparation, 62

Index

Thallium, ash temperature, graphite furnace, 518

Thermal analysis, 23-28 dielectric analyzer, 28 differential photocalorimetry, 24 differential scanning calorimetry, 24 diffusivity,27 dynamic mechanical analysis, 26-27 heat deflection temperature, vicat

softening point, 23-24 thermal conductivity, 27 thermogravimetric analysis, 25 thermomechanical analyzers,

dilatometers, 25-26 Thermal conductivity, 27, 129-154

amorphous materials, 143-145 ASTM standards, 132 chemical reaction, effect of, 149 comparative method, 135-137 composition, effect of, 147-149 crystallinity, effect of, 146 detector, gas chromatography, 368 guarded hot-plate technique,

132-133 heat flow meter, 132 heat-flow meters, 133-135 ISO standards, 132 laser-flash thermal diffusivity, 132,

140-141 line-source method, 132, 137-140 National Institute of Standards, 131 pressure, effect of, 147 standards, 131 thermal contact resistance, 141-143

Thermal desorption, gas chromatography, 387

Thermal diffusivity, 27, 149-151 Thermal gravimetric analysis,

modulated, thermogravimetric analysis of polymers, 123

Thermal stability, capillary rheometry, 73-74

Thermogravimetric analysis, 25, 111-128

applications, 117-123

Index

[Then a d

fi

n

n

r' t

cali c

op Then

api ap bu co

cu di1.

ex m 01 pi pi

tl tl

Index

illium, ash temperature, graphite furnace, 518

:rmal analysis, 23-28 ielectric analyzer, 28 ifferential photocalorimetry, 24 ifferential scanning calorimetry, 24 iffusivity, 27 ynamic mechanical analysis, 26-27 ~at deflection temperature, vicat

softening point, 23-24 iermal conductivity, 27 iermogravimetric analysis, 25 iermomechanical analyzers,

dilatometers, 25-26 rmal conductivity, 27,129-154 norphous materials, 143-145 STM standards, 132 iemical reaction, effect of, 149 imparative method, 135-137 Imposition, effect of, 147-149 ystallinity, effect of, 146 :tector, gas chromatography, 368 Larded hot-plate technique,

132-133 at flow meter, 132 at-flow meters, 133-135 o standards, 132 ser-flash thermal diffusivity, 132,

140-141 e-source method, 132, 137-140 ational Institute of Standards, 131 essure, effect of, 147 mdards, 131 ermal contact resistance, 141-143 mal desorption, gas

chromatography, 387 mal diffusivity, 27, 149-151 mal gravimetric analysis,

modulated, thermogravimetric analysis of polymers, 123

mal stability, capillary rheometry, 73-74

mogravimetric analysis, 25, 111-128

olications, 117-123

Index

[Thermogravimetric analysis] aging, physical, 119 degradation temperature,

determination of, 117-119 filler/additive content,

determination of, 121 modulated thermal gravimetric

analysis, 123 moisture determination,

119-120 reverse kinetics, 120-121 types of plastics in one sample,

determination of, 121-122 calibration techniques, 113-117

calcium oxalate monohydrate, measuring weight loss with temperature, 115-117

furnace calibration, 115 temperature calibration, 115 weight calibration, 113

operation principles, 111-113 Thermomechanical analysis, 155-200

applications, 174--194 applications of, 159-166 bulk measurement, 161-163 coefficient of thermal expansion,

159-161 cured thermosets, 174--184 dilatometry, 161-163 expansion, 159-161 mechanical tests, 165-166 operation of, 156-158 polymer melts, solutions, 184--188 pressure-volume-temperature

relationship, 163-164 theory, 156-158 thermoplastic solids, 174--184

glass transition, 177-178 rubbery plateau, 179-181 sub-T/dg/D transitions, 176-177 terminal region, 181 transition studies, frequency

dependencies in, 182-184 thermosets, 188-194

curing, 188-191

649

[Thermomechanical analysis] curing kinetics, by dynamic

mechanical analysis, 191-192 Gillham-Enns diagram, 193-194 photocuring, 191

Thermomechanical analyzers, dilatometers, 25-26

Thermoplastic solids dynamic mechanical analysis,

174--184 glass transition, 177-178 rubbery plateau, 179-181 sub-T/dg/D transitions, 176-177 terminal region, 181 transition studies, frequency

dependencies in, 182-184 Thermosets, dynamic mechanical

analysis, 188-194 curing, 188-191 curing kinetics by, 191-192 Gillham-Enns diagram, 193-194 photocuring, 191

Thermosetting polyesters, 587 Thin-layer chromatography, 12 Time-temperature superposition,

capillary rheometry, 72-73 Tin, ash temperature, graphite furnace,

518 Titration, automatic, 31 Torsion, vs. axial analyzers, dynamic

mechanical analysis, 173 Tungsten, temperature limits, 115 Turbidity, 40-41

Ultra-high-molecular-weight, 589 Ultraviolet-visible spectrophotometry,

17 Unsaturated polyesters, 275-276 Urea-formaldehyde resins, 279-281

Van Deemter curves, gas chromatography, 362

Vicat softening point, 23-24 Vinyl acetate-ethylene copolymer,

236-239

650

Vinyl chloride, polymers of, 242~248

Vinyl chloride-vinyl acetate copolymers, 243-245

Vinyl polymers with ester groups, 236--242

acrylate polymers, 24~242

methacrylate, 24~242

polyvinyl acetate, 236-239 polyvinyl alcohol, 239-240 vinyl acetate-ethylene copolymer,

236-239 Vinylidene chloride copolymers,

245-246 Viscosity detector, 13-14

Wet chemistry testing, 31-32 automatic titration, 3I chlorine analysis, 31-32 electrochemical analysis, 32

Index

[Wet chemistry testing) Ph/Ion measurements, 32

Window materials, infrared, optical properties of, 300

X-ray methods inorganic analyses, polymers, 512 polymer analysis, 512

Xylenol resin, 278

Zeeman interaction, 404-407 Zinc, ash temperature, graphite

furnace, 518 Zinc selenide, optical properties of,

300 Zinc sulfide, optical properties of,

300 Zirconia, cubic, optical properties of,

300