| SETTING UP YOUR EXPERIMENT | |||||
| Designing an NMR experiment: | |||||
| Number of scans:. | |||||
| As discussed previously, the Fourier-Transform approach to NMR utilizes a series of pulse-detect-wait sequences, the signals from which are added together in order to build up intensity. The number of times that this sequence is repeated obviously governs the total intensity of the final signal that is converted into an interpretable spectrum. As the free-induction decay (FID) builds up, the most obvious indication is the reduction of the noise (random signals holding no information) at long times, after the real signal has decayed away. Roll your mouse over the image below to see the effect on the FID of increasing the number of scans tenfold (from 10 to 100): | |||||
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| The difference in the signal-to-noise ratio (S/N) is also reflected in the final spectrum, as illustrated below: | |||||
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Unfortunately, one cannot simply double the number of scans in order to double the S/N, because the signal and the noise do not build up at the same rate. Instead, the signal increases as N1/2, where N is the number of scans. In other words, to double the signal, you need to quadruple the scans; to quadruple the signal, the number of scans must be increased by a factor of sixteen. Since the length of the experiment is directly proportional to the number of scans, this approach to enhancing the signal can quickly become extremely time-prohibitive. When running a 1H spectrum, the increase on going from, say, 16 scans (<2 minute experiment time) to 64 (about 5 minutes) to double S/N is not a particular hardship, but the same cannot be said for a typical 13C run (1024 scans with a 5 second pulse delay), which might increase from 1.5 to 6 hours. |
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The number of scans is one of the most commonly changed experimental parameters. Sample variables, such as concentration or viscosity, can make selection of a larger-than-standard number of scans advisable. In general, nuclides that are relatively rare (such as 13C at 1.1%, 15N at 0.37%, or 29Si at 4.7%) require much longer experiment times than those that are naturally abundant (such as 1H at 99.99%, and 31P and 19F at 100%) at the same concentration. Furthermore, those with lower Larmor frequencies (like 15N, 35Cl, or 23Mg) are inherently less sensitive than those which resonate higher (like 1H, 3H, or 19F), and there are other factors that can affect the sensitivity as well. To learn the fundamental NMR properties of a particular nuclide, consult an NMR Periodic Table. |
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