During preparation of acrylonitrile-1-d, CH<sub>2</sub>=CHD—CN, by D<sub>2</sub>O exchange, as described by Leitch (1), it was found that a linear relationship obtained between absorbance values for the 1165 cm<sup>−1</sup> band and the degree of exchange indicated by mass spectrometer data. This note contains a brief description of the exchange experiment, spectra of acrylonitrile before and after deuteration, and a table of IR and mass spectral data recorded at intervals during the exchange.

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