核磁经典教程 Understanding NMR Spectroscopy Keeler_ch5.pdfVIP

5 How the spectrometer works NMR spectrometers have now become very complex instruments capable of performing an almost limitless number of sophisticated experiments. How- ever, the really important parts of the spectrometer are not that complex to understand in outline, and it is certainly helpful when using the spectrometer to have some understanding of how it works. Broken down to its simplest form, the spectrometer consists of the follow- ing components: • An intense, homogeneous and stable magnetic field • A “probe” which enables the coils used to excite and detect the signal to be placed close to the sample • A high-power RF transmitter capable of delivering short pulses • A sensitive receiver to amplify the NMR signals • A digitizer to convert the NMR signals into a form which can be stored in computer memory • A “pulse programmer” to produce precisely times pulses and delays • A computer to control everything and to process the data We will consider each of these in turn. 5.1 The magnet Modern NMR spectrometers use persistent superconducting magnets to gen- erate the B0 field. Basically such a magnet consists of a coil of wire through which a current passes, thereby generating a magnetic field. The wire is of a special construction such that at low temperatures (less than 6 K, typically) the resistance goes to zero – that is the wire is superconducting. Thus, once the current is set running in the coil it will persist for ever, thereby generating a magnetic field without the need for further electrical power. Superconducting magnets tend to be very stable and so are very useful for NMR. To maintain the wire in its superconducting state the coil is immersed in a bath of liquid helium. Surrounding this is usually a “heat shield” kept at 77 K by contact with a bath of liquid nitrogen; this reduces the amount of (expensive) liquid helium which boils