Solvent gradient interaction chromatography
(SGIC) (cont.)
preparatory investigations, 108
HT-HPLC (see High temperature-high
performance liquid chromatography
(HT-HPLC))
limitations, 111
T
Temperature gradient interaction
chromatography
ethylene-octene copolymer separation
aim, 113, 115
equipment, 116
experimental set-up, 112, 114
materials, 115–116
measurement and evaluation, 117–118
mechanism, 112–114
preparatory investigations, 116
experimental variables, 115
Temperature rising elution fractionation
(TREF), 5–6
analytical and preparative scale, 12
block composition, 15
block index methodology, 18
chain folding, 17
column supports, 12
copolymer molecules, 17–18
cross-fractionation techniques, 19–21
crystallization, 12–13
dissolution/elution
crystallizability, 15
ethylene copolymers, 15–16
IR detector, 16, 17
monitoring, 15
α-olefin content, 15
soluble fraction, 13
solvent flow rate, 13
temperatures, 12
EO copolymers (see Ethylene-octene
(EO) copolymers)
EP copolymerization, 18–19
equipment, 38–39
Flory–Huggins statistical thermodynamic
theory, 12
FTIR/NMR, 16
high boiling point solvents, 12
hybrid 3D-SEC-TREF system 2, 20
impact polypropylene copolymers (see
Impact polypropylene copolymers
(IPCs))
instruments, 14, 15
molar mass fractionation, 19
Raman technique, LAM mode, 17
scanning calorimetry, 16, 17
SEC-TREF approach, 19, 20
size exclusion chromatography, 16, 17
thermo-oxidative degradation
compositional heterogeneity, 40–41
degraded bulk samples, 41–42
degraded samples, 42–46
non-degraded samples, 39–41
tacticity distribution, 18
TREF-SEC approach, 19, 20
X-ray diffraction, 16, 17
Thermal field-flow fractionation (ThF3), 147
Thermo-oxidative degradation, HT-AF4
aim, 162
equipments, 162–163
initiation reaction, 161
materials, 162
measurement and evaluation, 163–171
propagation reactions, 161
termination reactions, 161
Thermo-oxidatively degraded polypropylene
accelerated oven ageing, 36, 38
aim, 36
initiation reaction, 35–36
polymers, 36, 37
propagation reactions, 36
TREF fractionation
compositional heterogeneity, 40–41
degraded samples, 41–46
non-degraded samples, 39–41
Two-dimensional liquid chromatography
automated cross-fractionation instrument,
119
automatic TREF-SEC instrument, 119
EPDM sample, TGIC-SEC analysis of, 119,
120
EVA copolymer analysis
aim, 126
equipment, 126–127
materials, 126
measurement and evaluation, 127–129
preliminary investigations, 127
Hypercarb and 1-decanol-TCB, 119
IPC analysis
aim, 130
components, 129
equipment, 131–132
materials, 130
measurement and evaluation, 134–142
MMD and CCD, 129, 130
preliminary investigations, 132–134
178
Index
(SGIC) (cont.)
preparatory investigations, 108
HT-HPLC (see High temperature-high
performance liquid chromatography
(HT-HPLC))
limitations, 111
T
Temperature gradient interaction
chromatography
ethylene-octene copolymer separation
aim, 113, 115
equipment, 116
experimental set-up, 112, 114
materials, 115–116
measurement and evaluation, 117–118
mechanism, 112–114
preparatory investigations, 116
experimental variables, 115
Temperature rising elution fractionation
(TREF), 5–6
analytical and preparative scale, 12
block composition, 15
block index methodology, 18
chain folding, 17
column supports, 12
copolymer molecules, 17–18
cross-fractionation techniques, 19–21
crystallization, 12–13
dissolution/elution
crystallizability, 15
ethylene copolymers, 15–16
IR detector, 16, 17
monitoring, 15
α-olefin content, 15
soluble fraction, 13
solvent flow rate, 13
temperatures, 12
EO copolymers (see Ethylene-octene
(EO) copolymers)
EP copolymerization, 18–19
equipment, 38–39
Flory–Huggins statistical thermodynamic
theory, 12
FTIR/NMR, 16
high boiling point solvents, 12
hybrid 3D-SEC-TREF system 2, 20
impact polypropylene copolymers (see
Impact polypropylene copolymers
(IPCs))
instruments, 14, 15
molar mass fractionation, 19
Raman technique, LAM mode, 17
scanning calorimetry, 16, 17
SEC-TREF approach, 19, 20
size exclusion chromatography, 16, 17
thermo-oxidative degradation
compositional heterogeneity, 40–41
degraded bulk samples, 41–42
degraded samples, 42–46
non-degraded samples, 39–41
tacticity distribution, 18
TREF-SEC approach, 19, 20
X-ray diffraction, 16, 17
Thermal field-flow fractionation (ThF3), 147
Thermo-oxidative degradation, HT-AF4
aim, 162
equipments, 162–163
initiation reaction, 161
materials, 162
measurement and evaluation, 163–171
propagation reactions, 161
termination reactions, 161
Thermo-oxidatively degraded polypropylene
accelerated oven ageing, 36, 38
aim, 36
initiation reaction, 35–36
polymers, 36, 37
propagation reactions, 36
TREF fractionation
compositional heterogeneity, 40–41
degraded samples, 41–46
non-degraded samples, 39–41
Two-dimensional liquid chromatography
automated cross-fractionation instrument,
119
automatic TREF-SEC instrument, 119
EPDM sample, TGIC-SEC analysis of, 119,
120
EVA copolymer analysis
aim, 126
equipment, 126–127
materials, 126
measurement and evaluation, 127–129
preliminary investigations, 127
Hypercarb and 1-decanol-TCB, 119
IPC analysis
aim, 130
components, 129
equipment, 131–132
materials, 130
measurement and evaluation, 134–142
MMD and CCD, 129, 130
preliminary investigations, 132–134
178
Index