6 BRUKER BIOSPIN User Manual Version 002
Contents
16.2.5 T1p Relaxation Measurements .................................................................................... 209
16.3 Indirect Relaxation Measurements ............................................................................. 210
16.3.1 Indirect Proton T1 Measurements ............................................................................... 211
17 Basic MQ-MAS ....................................................................................213
17.1 Introduction ............................................................................................................... 213
17.2 Pulse sequences ....................................................................................................... 213
17.3 Data Acquisition ........................................................................................................ 215
17.3.1 Setting Up the Experiment .......................................................................................... 215
17.3.2 Two Dimensional Data Acquisition .............................................................................. 220
17.4 Data processing ......................................................................................................... 222
17.5 Obtaining Information from Spectra ............................................................................ 225
18 MQ-MAS: Sensitivity Enhancement ...................................................231
18.1 Split-t1 Experiments and Shifted Echo Acquisition ...................................................... 231
18.2 Implementation of DFS into MQMAS Experiments ...................................................... 233
18.2.1 Optimization of the Double Frequency Sweep (DFS) ................................................... 233
18.2.2 2D Data Acquisition .................................................................................................... 238
18.2.3 Data Processing .........................................................................................................240
18.3 Fast Amplitude Modulation - FAM .............................................................................. 242
18.4 Soft Pulse Added Mixing - SPAM ............................................................................... 242
19 STMAS ................................................................................................245
19.1 Experimental Particularities and Prerequisites ............................................................ 245
19.2 Pulse Sequences ....................................................................................................... 247
19.3 Experiment Setup ...................................................................................................... 249
19.3.1 Setting Up the Experiment .......................................................................................... 249
19.3.2 Two Dimensional Data Acquisition .............................................................................. 251
19.4 Data Processing ........................................................................................................ 253
20 Double-CP ..........................................................................................255
20.1 Pulse Sequence Diagram, Double CP (DCP) ............................................................. 256
20.2 Double CP Experiment Setup ..................................................................................... 256
20.2.1 Double CP 2D Experiment Setup ................................................................................ 256
20.2.2 15N Channel Setup .................................................................................................... 258
20.2.3 Setup of the Double CP Experiment ............................................................................ 259
20.2.4 Setup of the 2D Double CP Experiment ...................................................................... 264
20.3 2D Data Acquisition ................................................................................................... 265
20.4 Spectral Processing ................................................................................................... 266
20.5 Example Spectra ....................................................................................................... 267
21 CRAMPS: General ..............................................................................271
21.1 Homonuclear Dipolar Interactions .............................................................................. 271
21.2 Multiple Pulse Sequences .......................................................................................... 271
21.3 W-PMLG and DUMBO ............................................................................................... 272
21.4 Quadrature Detection and Chemical Shift Scaling ...................................................... 273
22 CRAMPS 1D ........................................................................................275
22.1 Pulse Sequence Diagram of W-PMLG or DUMBO ...................................................... 275