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A peak-search technique has been developed and evaluated for an automatic diffractometer. The instrument is a Buerger-Supper diffractometer with analyzing electronics and is driven through an IBM 1710 control computer. Indices and angular settings are precomputed and stored. After stepping to  γ ( hkl ) and  ϕ ( hkl ), 0.5 second counts are made at fixed increments of  Δϕ  on either side of the computed  ϕ  positions. From the  ϕ  search, scan rates and background-counting times are computed to give desired accuracy. The peak width and background positions are determined from second-order differences and curvatures computed from the peak half-height outward on either side of the peak. The background positions are accurately located on the radiation streak at all 2  θ  angles with an  ω  search and it is not necessary to use monochromators or balanced filters. A check method uses the search data to compute an alternate width to be used if necessary when  μ / γ  is large or when peak shapes are unusual.

A peak-search method for automatic diffractometry