11 Pulse NMR Spectroscopy英文电子书.pdf

- 1 1 - Pulse NMR Spectroscopy 11.1 INTRODUCTION TO THE PULSE NMR SPECTROSCOPY As we have seen before, we have to collect many spectra in order to observe signals from the carbon atoms of the organic molecules. An average time to sweep the proton absorption range (ca. 10 ppm) is 5 min. This would require more than 8 h in order to collect 100 NMR spectra. In the case of ^^C-NMR spectra it will take more time since we scan a range of 250 ppm and we have to collect more spectra than in proton NMR. What can we do in order to shorten the length of time to collect 100 NMR spectra? As mentioned in the ^H-NMR section, CW spectrometers use either a frequency-sweep technique or field-sweep technique. By the application of such techniques, each different kind of proton (or carbon) must be brought into resonance one by one and any change in the absorption will be recorded. The question is how can we shorten the time that is necessary for one scan. For example, we can increase the rate of scans from 5 to 1 min, but this would result in a decrease in resolution. Fast scanning is not a solution. The pulse technique was developed largely in response to the need for much higher sensitivity. This higher sensitivity is achieved by simultaneously exciting all of the nuclei. With this technique, scanning time is decreased from 5 min to a few seconds. Nowadays, one can collect up to 1000 scans in 10-1 5 min. This mode is called Fourier transform spectroscopy. Let us compare the CW (continuous wave) and FT (Fourier transform) techniques. 11.2 CW AN D FT SPECTROSCOPY In the conventional CW NMR experiment, a radiofrequency field is continuously applied to a sample in a m