A new experiment for the single‐scan measurement of diffusion coefficients is presented. The principle is to introduce a spatial variation in the parameters of a conventional pulse sequence, so that all of the scans required to determine some physical parameter can be recorded simultaneously from different parts of the sample. The spectrum is acquired in the presence of a weak read gradient so that the resulting lineshapes contain the information required. The pulse sequence is described in detail and demonstrated on a sample containing three components; its advantages and limitations are discussed in relation to those of existing techniques. For uncrowded spectra with high signal‐to‐noise ratio, this experiment provides an order of magnitude reduction in experiment time compared with conventional methods and is likely to be of most benefit where samples are changing rapidly with time or where a long period of polarization, which may be difficult to reproduce accurately, prohibits the use of multiple‐scan techniques. Copyright © 2003 John Wiley & Sons, Ltd.