User Manual Version 002 BRUKER BIOSPIN 3
Contents
Contents ............................................................................................... 3
1 Introduction ........................................................................................... 9
1.1 Disclaimer .................................................................................................................... 10
1.2 Safety Issues ............................................................................................................... 10
1.3 Contact for Additional Technical Assistance .................................................................. 10
2 Test Samples ........................................................................................11
3 General Hardware Setup ..................................................................... 15
3.1 Connections to the Preamplifier .................................................................................... 15
3.2 RF Connections Between Preamplifier and Probe ......................................................... 20
3.3 RF-Filters in the RF Pathway ........................................................................................ 21
3.4 Connections for Probe Identification and Spin Detection ............................................... 25
3.5 MAS Tubing Connections ............................................................................................. 26
3.5.1 Connections ..................................................................................................................27
Wide Bore (WB) Magnet Probes ...............................................................................28
Standard Bore (SB) Magnet Probes ..........................................................................30
3.6 Additional Connections for VT Operation ...................................................................... 31
3.7 Probe Setup, Operations, Probe Modifiers .................................................................... 41
3.7.1 Setting the Frequency Range of a Wideline (single frequency) Probe ............................41
3.7.2 Shifting the Probe Tuning Range ...................................................................................42
3.7.3 Adding a Frequency Channel to a Probe (WB probes only) ............................................48
3.8 Mounting the Probe in the Magnet/Shim Stack .............................................................. 50
3.9 EDASP Display: Software Controlled Routing ............................................................... 51
4 Basic Setup Procedures ...................................................................... 55
4.1 General Remarks ......................................................................................................... 56
4.2 Setting the Magic Angle on KBr .................................................................................... 57
4.2.1 RF-Routing ...................................................................................................................57
4.2.2 Setting Acquisition Parameters ......................................................................................59
4.3 Calibrating 1H Pulses on Adamantane .......................................................................... 65
4.4 Calibrating 13C Pulses on Adamantane and Shimming the Probe ................................. 73
4.5 Calibrating Chemical Shifts on Adamantane ................................................................. 75
4.6 Setting Up for Cross Polarization on Adamantane ........................................................ 76
4.7 Cross Polarization Setup and Optimization for a Real Solid: Glycine ............................. 79
4.8 Some Practical Hints for CPMAS Spectroscopy ............................................................ 85
4.9 Field Setting and Shift Calibration ................................................................................ 87
4.10 Literature ..................................................................................................................... 88
5 Decoupling Techniques ...................................................................... 89
5.1 Heteronuclear Decoupling ............................................................................................ 89
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