Molecular Sieves - Science and Technology - Vol. 6 - Characterization II / 07-back-matter

–, interferences, 35

–, mathematically calculation, 35 –, matrix effects, 36

–, photoelectric absorption, 33 –, sample preparation, 36

–, standard deviation, 36

–, wavelength dispersive (WD) mode, 34 –, XRF spectrum of SAPO-11, 34

X-ray Photoelectron Spectroscopy (XPS), 61

–, characterization of the surface region, 61

–, charging of the insulating sample, 61 –, framework, 61

–, non-framework, 61

X-ray powder diffraction, 52 –, cation loading, 52

–, symmetry of the crystal lattice, 52

129Xe

–, chemical shift, 160 –, hyperpolarized, 159

–, natural abundance, 159 –, nonzero spin, 159

–, resonance, 159

–, sensitivity of detection, 159

–, spin relaxation time T1, 159, 160 129Xe 1D NMR spectrum

–, xenon adsorbed on Na-A zeolite, 218 129Xe 2D exchange NMR

–, from one cage to another, 219 129Xe 2D exchange NMR spectrum

–, xenon adsorbed on Na-A zeolite, 218 129Xe 2D exchange NMR spectrum

–, of xenon adsorbed on V2O5, 233 129Xe 2D spectra

–, cage occupancy, 220 –, diffusivity, 220

129Xe cage-to-cage migration –, activation energy, 175

129Xe chemical shift

–, dynamics of adsorbed xenon, 214 –, exchange interactions of the wave

functions, 162

–, location of transport resistance, 214 –, site occupancy, 219

–, site-to-site exchange, 219 Xe density

–, amagat, 162 129Xe in solvents

–, gas to solution shifts of, 161

Xe NMR

–, in the presence of an active gas, 166 129Xe NMR

–, characteristics of void spaces, 163 129Xe NMR investigations

–, adsorbed organic molecules, 194

–, adsorbed Xe at high temperature and pressure, 217

–, adsorption of benzene, 198 –, adsorption of CO, 209

–, adsorption of H2 on O2 , 209

–, adsorption of H2 on Pt/Al2O3, 209

–, adsorption of Mo(CO)6 in zeolite Na–Y, 210

–, adsorption of O2 on Pt/Al2O3, 209 –, Al2O3 , 232

–, Al2O3 –ZrO2, 232

–, AlPO4-8 structure in a VPI-5 sample, 182 –, bulk, 194

–, calculations, 170

–, cation exchange between different zeolites, 191

–, Cd–Rho, 181

–, channel blockage by coke deposition, 201 –, characterization of coke on zeolites, 297 –, charge on AlNF, 194

–, chemisorption, 204

–, chemisorption of hydrogen, 205

–, chemisorption on supported metal particles, 205

–, cloverite, 181

–, coke between zeolite crystallites, 200 –, coke distribution, 202

–, coke formation, 200 –, coke location, 201

–, coking of HY zeolites, 203 –, combination of ESR, 189

–, combined with 1H pulsed-field gradient NMR, 203

–, combined with argon sorption measurements, 203

–, combined with multiple-quantum NMR spectroscopy, 196

–, CoNa-Y, 186

–, correction of the magnetic susceptibility, 161

–, cracking activity, 200 –, crystallinity, 181, 182 –, deactivation, 201

–, dealuminated Y zeolite, 182

–, decomposition of Pt(NH3)2+4 complex, 209

–, dehydration, 185

–, dehydration of La3+ and Ce3+ exchanged Y, 186

–, dehydration of Na–Y, 199

–, determination of the particle size, 205

–, diffusion of an adsorbate in a zeolite, 185 –, diffusion of H2O in 13 X zeolite, 221

–, diffusion of H2O in NiNa–Y, 221 –, dispersed Mo2 clusters, 210

–, distribution of adsorbed phases, 194 –, distribution of benzene in Na–X and

Na–Y, 197

–, distribution of clusters in Y crystallites, 208

–, distribution of gas, 209

–, distribution of phases chemisorbed, 205 –, distribution of Ni2+ cations, 185

–, distribution of Xe atoms among α-cages of Na–A, 217

–, effect of binder, 216

–, effect of nonframework aluminum, 193 –, exchange of cations between different

zeolites, 192

–, ferrierite-mordenite intergrowth, 182

–, gases chemisorbed on zeolite-supported metal particles, 210

–, H–Cs–Rho, 181

–, homogeneity of industrial samples, 217 –, hydrocarbon chains attached to silica

walls, 235

–, hydrogen atoms adsorbed on Pt clusters, 207

–, HZSM-5 coking, 201

–, industrial catalysts, 216

–, influence of an adsorbate on the spectrum of xenon coadsorbed as a probe, 221

–, influence of trivalent cations, 186 –, intercrytalline exchange of guest

molecules, 223

–, intracrystalline concentration profiles, 221

–, intracrystalline transport diffusion, 221 –, Lennard-Jones potential curves, 170, 171 –, list of applications, 238

–, location and oxidation state of cations, 185

–, mesopore voids, 235

–, mesoporous silica, 235 –, Mg70-Y, 185

–, molecules on Pt, 209 –, mordenite, 181, 182

–, mutual hindrance xenon atoms/benzene molecules, 198

–, Na–A/Xe system, 217

–, number of atoms per Pt particle, 208 –, number of Pt atoms per metal particle,

207

–, offretite-erionite intergrowths, 182 –, paramagnetic cations, 185

–, physical interaction Xe atom/surface consisting of oxygen atoms, 170

–, platinum supported on alumina, 209 –, porous carbons, 227, 228

–, Pt clusters inside mesoporous molecular sieve, 235

–, Pt–H/Na–Y crystallites, 217

–, quantum chemical ab-initio calculations, 189

–, reduction and reoxidation of Ni7.5Na-Y, 185

–, reduction/oxidation processes of copper ions, 189

–, rehydration, 185

–, reoxidation of coked zeolites, 202

–, role of extra-framework aluminum, 200 –, Ru3+ ions in Y, 186

–, secondary porosity, 182

–, self-diffusion coefficient of xenon in Pt–Na–Y, 217

–, shielding constant, 160

–, silica-based materials, 231

–, sizes of micropores inside the mesopore walls, 235

–, sorbate dynamics, 218 –, sorbate location, 218

–, study of chemisorption, 203 –, study of coke deposition, 199 –, study of supported metals, 203

–, study of the H2 O/Na–Y system, 198

–, study of various Pt/Na–Y samples, 207 –, studying bimetallic catalysts, 210

–, temperature dependence, 163

–, V2O5, 232

–, van der Waals interactions, 161

–, Xe adsorbed in microor meso-cavities of coke, 201

–, Xe–O interaction, 170

–, xenon adsorbed on Ptx-Na-Y, 205 –, Y zeolite, 182

–, Y3+ exchanged in Y, 186 –, zeolite intergrowths, 181

–, zeolite monolayer on a surface, 238 –, ZSM-5, 182

–, ZSM-5-ZSM-11 intergrowth, 182 129Xe NMR chemical shift

–, Beta, 179 –, EU-1, 179

–, function of cage radius, 171 –, LZY-52, 179

–, MAPO-36, 179

–, SAPO-41, 179

–, second virial coefficients, 163 –, silicalite-1, 179

–, surface-induced NMR chemical shift, 169 –, variation versus Al content of the

framework, 178

–, VPI-5, 179

–, 129Xe trapped in a variety of zeolites, 169 –, ZK-4, 179

–, ZSM-23, 179

129Xe NMR chemical shift, 163

–, adsorption isotherms of Xe in transition metal ion-exchanged zeolites (Ag, Cu, Zn, Cd), 190

–, aerosil, 229

–, after dealumination, 180

–, Ag+–Xe complex, 188

–, Ag+, Cu+, Zn2+, and Cd2+ cations, 187 –, Ag–X, 187, 188

–, Ag-Y, 190

–, AlPO4-5, 178 –, AlPO4-11, 180 –, AlPO4-5, 180

–, as a function of the cation exchange degree, 183

–, beta zeolite, 180

–, calculated chemical shift, 172 –, calculations, 171

–, CdX, 188

–, contact overlap, 164 –, Cu-X, 188

–, Cu-Y, 188

–, dependence on the chemical composition, 178

–, dependence on the xenon concentration, 179

–, diamagnetic and paramagnetic ions, 184

–, different Si/Al ratio, 184 –, discussion of models, 172 –, due to the porosity, 166

–, effect of H and alkali-metal ions, 183 –, effect of the electrical field, 165

–, extra-framework species, 178 –, fast site exchange model, 167 –, faujasite, 178

–, function of mean free path in various zeolites, 177

–, function of temperature, 171, 173, 174 –, function of the total Xe concentration,

168

–, function of xenon concentration, 164 –, H-Y, 184

–, in mixtures of xenon and other gases, 163 –, influence of cations, 183

–, influence of divalent cations, 184 –, influence of surface curvature, 168 –, interaction Xe/surface, 164

–, interaction Xe–Xe, 164

–, intercrystallite exchange, 173 –, internal free volume, 179

–, internal void volume space, 180 –, L, 180

–, large shift induced by gaseous O2 and NO, 164

–, location of cations, 183

–, mean free path of a Xe atom, 166 –, Mg-Y, 184

–, migration of cations, 183

–, model of xenon adsorption, 190 –, models, 173

–, models for the interpretation, 166

–, molecular dynamics simulations, 172 –, molecular interaction energy with the

surface, 169

–, multivalent cations, 168 –, Na-Y, 166, 184

–, paramagnetic cations, 165 –, pore diameters, 180

–, porosity studies, 175 –, porous silica, 231

–, quantitative dependence on the concentration of sorbed xenon, 190

–, related to the structure, 179 –, SAPO-5, 178, 180

–, SAPO-11, 180

–, SAPO-34, 180

–, SAPO-37, 178, 180

–, series of zincand cadmium-exchanged Y zeolites, 191

–, Si/Al ratio, 180 –, silica, 229

–, statistical models, 174 –, strong adsorption, 168

–, strong adsorption sites (SAS), 165 –, sum of several terms, 164

–, supported metals, 168

–, temperature of thermal treatment, 183 –, theoretical approach, 191

–, Theta, 180

–, void volume, 165 –, VPI-5, 180

–, weak adsorption, 168

–, Xe diffusion rate constants in zeolites, 173

–, xenon mobility, 173 –, Y zeolites, 180

–, zeolite A, 173

–, zeolite Na-A, 174 –, zeolite Na-Y, 174

–, zeolite with a single type of void volume, 179

–, zeolite X with cations, 183 –, zeolite Y, 173

–, zeolite Y with cations, 183 –, zeolite ZSM-5, 173

–, Zn-X, 188 –, ZSM, 180

–, ZSM-11, 178

–, ZSM-5, 166, 178

Xe NMR cryoporometry

–, determination of pore dimensions, 235 –, lowered melting point of the confined

substance, 236

–, mesoporous materials, 236 –, pore size, 236

–, pore size distribution, 237 129Xe NMR data

–, multisite magnetization transfer experiments, 175

–, two-dimensional exchange NMR, 175 –, xenon trapped in α-cages of Na-A, 175 129Xe NMR quantitative spectroscopy

–, location and number of cations, 189 129Xe NMR shift of adsorbed xenon

–, correlation with 1H PFG NMR of

hydrocarbons, 215 129Xe NMR spectra

–, chemisorbed hydrogen, 206

–, during the sorption of benzene on crystallites of ZSM-5, 222

–, ferrierite, 180

–, in Na-Y zeolite with loading of 0.5 HMB, 195

–, possible dispersion of guest molecules among cavities, 195

–, xenon adsorbed on Pt–H–Na-Y, 206 –, zeolite Cs–Rho, 180

–, zeolite H–Rho, 180 –, zeolite Rho, 180

–, zeolites with several types of void

volume, 180

129Xe NMR spectroscopy

–, 12-tungstophosphoric heteropolyacids (HPA), 225

–, heteropoly acids (HPA), 226

–, heteropolyoxometalate salts (HPOM), 225

129Xe NMR spectrum of xenon

–, adsorbed on Ptx–H–Na-Y after heat

treatment, 208 129Xe NMR study

–, employing the Xe-131 isotope, 233

–, of aerogels, 233

129Xe NMR technique

–, amorphous oxides, 228 129Xe NMR

–, virial expansion of the xenon density, 162 129Xe PFG NMR

–, in Na–X zeolite, 212 129Xe polarization

–, applications of, 240 129Xe spectroscopy

–, interlayer spacing, 224 –, study of PILC, 224

Xe-NMR of adsorbed xenon –, applications, 237

Xenon (see especially 129Xe) –, isotopes, 159

–, natural abundance, 159 –, NMR properties, 159

Xenon derivatives –, 129Xe NMR, 160

Xenon diffusion

–, from one cage to another, 219 Xenon hyperpolarization, 238 Xenon porometry

–, determination of pore dimensions, 235

XPS

–, bulk composition, 63 –, dealumination, 63

–, surface composition, 63 Xylene isomerization

–, pre-coking, 349

–, pre-coking/post-modification treatment, 349

–, selective passivation of the external active sites, 349

Zeolite A

–, adsorption capacities, 115

–, coiling of high molecular weight alkanes, 124

–, Xe adsorbed in, 217 Zeolite A (LTA)

–, pore size, 121 Zeolite Ba-X

–, pore size characterization, 125 Zeolite Beta

–, acidity of [Fe]-Beta, 91 –, coke formation, 73

–, crystallized in alkaline media, 85

–, decomposition of the TEA+ cations, 85 –, in Ga-, Fe-variants, 91

–, Pt–Pd particles, 63

–, removal of TEA-OH, 85 –, TEA+ decomposition, 91 –, TG, 85

–, thermal behavior of as-synthesized Beta, 85

–, thermal decomposition of TEA, 87 –, XPS spectroscopy, 63

Zeolite Ca-X

–, pore size characterization, 125 Zeolite Ca-Y

–, pore size characterization, 125

Zeolite Cs–Rho

–, 129Xe NMR spectra, 180 Zeolite Cs-X

–, pore size characterization, 125

Zeolite H–Rho

–, 129Xe NMR spectra, 180 Zeolite H-MCM-22 (MWW) –, m-xylene reactions, 135 Zeolite H-ZSM-5

–, 2-methylnaphthalene/1- methylnaphthalene mixture on, 124

–, adsorption of xylenes, 124

–, competitive adsorption of n-alkanes and aromatics on, 124

Zeolite H-ZSM-12

–, 2-methylnaphthalene/1- methylnaphthalene over, 125

Zeolite intergrowths, crystallinity –, 129Xe NMR, 181

–, zeolite composition, 181 Zeolite ITQ-4 (IFR)

–, micropore volume, 114

–, packing density of m-xylene, 114 –, probing the pore size, 114 Zeolite K-A

–, pore size, 121 Zeolite Li-X

–, pore size characterization, 125 Zeolite MCM-22 (MWW)

–, adsorption capacities for n-hexane, cyclohexane, m-xylene and mesitylene, 125

–, adsorption isotherms, 125

–, characterized by adsorption, 125 Zeolite MFI, 123

–, adsorption properties of, 123 Zeolite Na-A

–, pore size, 122 Zeolite Na-X

–, pore size characterization, 125 Zeolite Na-Y

–, 2-methylnaphthalene/1- methylnaphthalene over, 125

Zeolite omega

–, thermal decomposition of the template, 82

Zeolite Rho

–, flexibility of this structure, 181 –, 129Xe NMR spectra, 180, 181

Zeolite structures

–, combined XPS and ISS (ion-scattering spectroscopy), 63

Zeolite UTD-1 (DON)

–, adsorption capacities, 114 Zeolite VPI-5

–, adsorption of 1,3,5-triisopropylbenzene, 126

Zeolite with a single type of void volume –, diffusion of xenon, 179

–, internal free volume, 179 –, single line, 179

–, 129Xe NMR chemical shift, 179 Zeolite Y

–, coiling of high molecular weight alkanes, 124

Zeolite ZSM-5

–, disproportionation of m-xylene, 133 –, isomerization of m-xylene, 133 Zeolites, 3, 4

–, chemical composition, 3 –, definition, 3

–, general compositional formula, 3 –, quantitative analysis, 4

–, spatial distribution, 4

–, void spaces by 129Xe NMR, 163 –, 129Xe NMR chemical shift, 180

–, 129Xe NMR chemical shift as a function of mean free path, 177

Zeolites (metal-loaded) –, chemisorption, 204 Zeolites L (LTL)

–, m-xylene test reaction, 136

Zeolites with divalent cations –, 129Xe NMR, 184

Zeolites with H and alkali metal ions –, 129Xe NMR, 183

Zeolites with several types of void volume –, 129Xe NMR spectra, 180

Zeolites with transition metal cations –, 129Xe NMR, 187

Zeolites with trivalent cations –, 129Xe NMR, 186

Zeolites Y (FAU)

–, adsorption capacities, 114 –, m-xylene test reaction, 136

Zincoaluminonophosphates, 372 Zincoarsenates, 371 Zincophosphates, 371 Zincosilicate samples

–, IR spectra (KBr pellets), 456

–, scanning electron micrograph, 456 –, XRD patterns, 456

Zincosilicates, 371

–, catalytic activity, 459 –, cyclar process, 372 –, in methanol, 372

–, ion exchange, 459

–, modified with copper, 372 –, Raman spectra, 459

–, redox activity, 372

–, 29Si MAS NMR spectra, 459 ZK-5

–, pores of, 121 [Zn]-MFI

–, by conventional hydrothermal synthesis, 459

–, crystallinity, 455 –, crystallization, 459 –, DTG peaks, 457

–, gel preparation, 385

–, introduced tetrahedral zinc, 457 –, ion-exchange ability, 457

–, IR spectra, 455 –, morphology, 455

–, Raman spectroscopy, 457 –, reducibility, 458

–, 29Si MAS NMR spectra, 459 –, structure defects, 458

–, synthesis procedure, 385

–, temperature of the DTG peaks, 458 –, temperature-programmed reduction

(TPR), 458

–, TPR profiles, 458 ZSM-11 (MEL)

–, adsorption behavior, 112 ZSM-5

–, coke formation, 73

–, desorption-decomposition features of propylamines, 97

–, templates, 78

ZSM-5 (copper-exchanged) –, 2-propylamine on, 95

–, TPD/TGA, 95 ZSM-5 (MFI)

–, adsorption behaviour, 112

–, multicomponent adsorption experiments on, 122

–, xylene isomers on, 122 ZSM-11

–, thermal analysis of, 78 ZSM-20

–, thermal decomposition of the template, 82

ZSM-23 (MTT)

–, adsorption behavior, 112 –, Constraint Index, 131 ZSM-35 structure

–, trimethyl-cetyl-ammonium, 84 ZSM-48

–, adsorption behavior, 112 ZSM-5

–, changes in unit cell parameters, 49 –, wavenumbers of lattice vibrations, 50