IV. Signal-to-Noise Measurement - II

Choice of a noise region must be consistently applied for standard samples, and for 0.1% ethylbenzene (ETB), we have chosen 5 to 3.5 ppm. It is also critical that the noise be amplified if necessary in order to make an accurate measurement using a ruler. There is not much point in

trying to compare the ratio of noise to a few millimeters high to a peak 20 cm high; plot the noise such that it is several centimeters high. If the instrument performs the signal-to-noise measurement and calculation, the relative intensities are not as critical. Both the Unity+300 and VXR-S 400 NMR spectrometers perform the S/N calculation by software commands.

The last point concerning sensitivity is demonstrated during the 13C{1H} part of the checkout. The checkout requires that you acquire three spectra, using 1, 4, and 16 transients. Signal-to-noise increases as the square root of the number of transients; to double the signal-to-noise you must take four times as many transients.

When using a concentrated sample such as 30% menthol for 13C, or when running routine 1H spectra, the number of transients or scans is quite small, so the point discussed above may not seem important. However, suppose you are in the following situation: you have only a few mg of research sample, and after collecting a 13C{1H} spectrum on the Unity+300 for 2 hours, you get peaks with S/N of only 5:1. Since the peaks are barely visible above the noise ( and you may have missed quarternary carbons), you want to re-collect the spectrum to get a S/N of 50:1, a value most typical for carbon NMR. Unfortunately, this will take 10x10x2 = 200 hours! In such cases, you should consider using a higher field strength spectrometer, which will be able to give you a spectrum with good S/N in much less time.

 

Reblog this post [with Zemanta]

No comments: