Negative ion mass spectra organic nitriles have been determined using 1 Torr of methane moderator/reagent gas in a chemical ionization source. The spectra contain abundant (<i>M</i> – 1)<sup>−</sup> ions, and fragmentations are minimal. Ion/molecule reactions with residual oxygen, methane, and between sample molecules and ions form diverse products with low abundances relative to the (<i>M</i> – 1)<sup>−</sup>. Detection limits are comparable with positive ion methods, and for selected compounds, can be several orders of magnitude lower.

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