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  • 核磁共振 定量_nmr_實驗條件要注意的問題和應用領域

    上一篇 / 下一篇  2010-09-29 14:16:21

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      核磁共振定量NMR 實驗

      實驗考慮:

      Good signal to noise 好的信燥比

      90° pulse sufficiently short to excite the entire region uniformly

      Delay between pulses of at least 5 T1’s 脈沖延遲至少T1的5倍

      Flat base line to start with and baseline correction 基線平坦和基線校正

      Filter bandwidth set to at least twice the sw

      Enough data points to give 15 to 20 points per peak - remember that you lose half the points to the imaginaries in Fourier transformation

      Acquire at least 32k and zero fill several times – memory is cheap

      Exception to 32k for other nuclei requiring 1H decoupling - it is important to limit the acquisition time to as short as possible to avoid NOE build up during the acquisition so < 32k may be necessary with zero filling to make up the difference

      Zero filling should only be done after dc correction and line broadening otherwise it introduces baseline artifacts

      Gated decoupling for non-hydrogen analysis

      Careful phasing on a spectrum that has been greatly expanded in the vertical direction

      Careful integration

      Place a single integral over the spectral limits of interest

      Adjust bias and slope on the full integral

      Cut integral into smaller regions as close as possible to the peak

      Consistently include or exclude satellites or account for them when they overlap




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