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A new X-ray diffraction method for the determination of the amount and distribution of fixed NH +  4  in illite-smectite has been developed. Illite-smectite was saturated with K +  and heated at 150 °C. The 002 and 005 reflections were recorded with steps of 0.01° 2θ, and the experimental d values and the values for full-width at half-height (FWHH) were determined using a peak-profile-fitting procedure. Peak profiles were calculated with the NEWMOD program for illite structures having different amounts of NH +  4  and different patterns for the distribution of NH +  4  in interlayers. For Upper Jurassic illite-smectite from North Sea oil source rocks, the amount and the distribution of NH +  4  in illite interlayers were determined by comparing the experimental values for d 005  and FWHH with the values calculated for the selected illite structures. The amounts of NH +  4  determined in this manner correlate well with the amounts determined by an isotopic dilution method. The results demonstrate that these illite-smectite samples have K end-member illite and NH 4  end- member illite (tobelite) layers and that the illite layers formed during diagenesis and oil generation actually are tobelite layers.

Determination of the content and distribution of fixed ammonium in illite-smectite by X-ray diffraction: Application to North Sea illite-smectite