NUS: non-uniform sampling
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- Cecily Logan
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1 FMP,
2 2/48 NMR-spectroscopy uses the nuclear spin that can be thought of as a mixture between gyroscope and magnet
3 3/48 The frequency of the rotation of the spin in a magnetic field is what we are interested in B 0 [Tesla] 0 [MHz]
4 4/48 The frequency is measured by using the little magnet to induce a current in a coil
5 5/48 An RF-pulse is used to start the magnet. Because of signal-tonoise we repeat the excitation-detection
6 6/48 While the frequency of one line is easy to analyze from the timesignal it is difficult from more than one
7 7/48 That s why we do a Fourier-Transformation! FT
8 8/48 For which we have to digitize the signal. Then we can use the DFT or FFT to process data fast.
9 9/48 1, Hz intensity 0,5 0-0,5 The DFT only sorts points ,005 0,01 0,015 0,02 0,025 0,03 0,035 0,04 time (sec) 1, Hz 0,8 FT intensity 0,6 0,4 0, frequency
10 10/48 The maximum frequency that we want to detect determines the sampling rate: Nyquist condition
11 11/48 What about resolution, i.e. separating two lines? To do that we have to sample many points!
12 12/48 This comes for free in a 1D! If t acq gets longer one can shorten t r
13 13/48 90 x k t 1 90 y k t2 A multidimensional 90 x k t 1 90 y k t 2 90 x k t 1 90 y k t 2 90 x k t 1 90 y k t 2 spectrum is created by repetitive recording of a one-dimensional spectrum with systematic changes in the pulse-sequence.
14 14/48.resulting in a two-dimensional FID
15 15/48 The first FT yields the interferogram
16 16/48 The second FT yields the two-dimensional spectrum
17 17/48 Spectra are usually viewed as contour plots
18 18/48 90 x k t 1 90 x k t 2 90 y k t 3 90 x 90 y has to be done in two In a 3D the repetition indirect dimensions independently 90 x k t 2 k t 3 k t 1 90 x 90 x 90 y k t k t 3 1 k t 2 90 x 90 x 90 y k t k t k t x 90 x 90 y k t k t 3 1 k t 2 90 x 90 x 90 y k t k t 3 1 k t 2
19 19/48 That is why multidimensional spectra take so much longer 1D, 1024 points, 8 scans 12 sec 2048 points do not (!!) take longer 2D, 1024 x 1024, 8 scans 4,3 hours 1024 x 2048 points take 8,6 hours 3D, 1024 x 128 x 128, 8 scans 54,6 hours 4D, 1024 x 32 x 32 x 32, 8 scans 109,2 hours 4D, 1024 x 128 x 128 x 128, 8 scans 291 days The reason is the DFT!
20 20/48 The DFT is fast but also has some limitations: Points have to be sampled in equidistant intervals The distance between points determines the maximum frequency that can be sampled Missing points at the beginning, in the end or in the center cause distortions Good resolution in nds requires long experiment time!!
21 21/48 indirect dimension all points
22 22/48 indirect dimension initial points missing
23 23/48 indirect dimension last points missing
24 24/48 indirect dimension points missing inbetween
25 25/48 Maximun-Entropy Reconstruction Multi-Dimensional Decomposition
26 26/48 exponentially-decaying signal indirect dimension J.C.J. Barna et al. J. Magn. Reson. 73, (1987)
27 27/48 sine-modulated signal (e.g. cosy-experiment) indirect dimension P. Schmieder et al. J. Biomolec. NMR 3, (1993)
28 28/48 non-decaying signal (e.g. ct-experiment) indirect dimension P. Schmieder et al. J. Biomolec. NMR 4, (1994)
29 29/48 In 3D there are two indirect dimensions 64 x 128 complex points
30 30/48 exponentially-decaying signals in 3D 512 out of 8192 (64 x 128) complex points A.S. Stern et al. J. Am. Chem. Soc. 124, (2002)
31 31/48 non-decaying signal in 3D 512 out of 8192 (64 x 128) complex points A.S. Stern et al. J. Am. Chem. Soc. 124, (2002)
32 DO2 HO 2 NUS: non-uniform sampling 32/48 sampling limit the sample provides sufficient S/N and the data have to be recorded far too long to achieve enough resolution NUS can drastically shorten the experiment time sensitivity limit the sample requires an extended experiment time to achieve a sufficient S/N anyway and the required resolution can easily be obtained NUS can provide more flexibility
33 33/48 ct-hnca of MHz We are clearly in the sampling limit! 13 C: the ct-delay is 27 msec, the increment is 132 sec we can collect 200 complex points (400 FIDs) 15 N: the ct-delay is 22 msec, the increment is 220 sec we can collect 100 complex points (200 FIDs) The full 3D would therefore consist of FIDs Assuming 4 scans and 0.8 sec relaxation delay this amounts to 80 hours, while 1 hour is enough for S/N!
34 34/48 ct-hnca of MHz Projections of a dataset with 100* x 200* = full points, i.e. 80 hours spectrometer time
35 35/48 ct-hnca of MHz if we cut this to 8 hours classically (32* x 64* = 2048 full points) we have less resolution
36 36/48 ct-hnca of MHz by cutting to 8 hours the sampling is drastically reduced: 32* x 64* = 2048 full points
37 37/48 ct-hnca of MHz 2048 out of (10.2%)
38 38/48 ct-hnca of MHz 8 hours instead of 80 traditional
39 39/48 ct-hnca of MHz 8 hours instead of 80 traditional
40 40/48 ct-hnca of MHz 256 out of (1.3%)
41 41/48 ct-hnca of MHz 256 out of : 1 hour instead of 80
42 42/48 Acquisition of NUS data in topspin 3.1
43 43/48 Acquisition of NUS data in topspin 3.1 NUSLIST is the sampling schedule, which can also be created independently (it is a vc-list) Parameter to creat the sampling schedule: NusAMOUNT gives the percentage of points (NusPOINTS) selected
44 44/ Acquisition of NUS data in topspin 3.1 The points in the NUSLIST are also ordered randomly so that reasonable processing is possible without waiting for the experiment to finish. The list is stored in the dataset under the name nuslist How many points have been recorded is stored in the parameter NusTD for each dimension while the TD only gives the maximum number of points
45 45/48 Acquisition of NUS data in topspin 3.1 Parameter to adjust the sampling schedule: NusJSP if a cosine-modulation due to coupling is present NusT2 if there is a decay due to relaxation
46 46/48 Acquisition of NUS data in topspin 3.1 using NusJSP and NusT2 t max = 20 msec J = 50 Hz 1/2J = 10 msec t max = 15 msec T 2 = 5 msec
47 47/48 Processing of NUS data in topspin 3.1 NUS is recognized by the command ftnd and mdd is started automatically ftnd 0
48 48/48 Thank you
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