X-ray diffraction data for seventeen 5α-pregnanes were collected using a General Electric XRD-5 diffractometer with a nickel-filtered CA-7 copper target tube operated at 40 kv and 20 ma in conjunction with a scintillation counter and a No. 2 SPG preamplifier. The linear scale of a Leeds and Northrup Speedomax G recorder was used to record the X-ray powder spectra. Samples were run at a speed of 0.2°/min using a take-off angle of 2.0°, a 3.0° beam slit, a medium resolution Soller slit, and a 0.1° detector slit. The number of cps was recorded by a digital printer that was synchronized with the 2θ scan. The digital tape readings and Speedomax charts were compared to determine maximum peak heights and locations in accordance with the accepted methods outlined by Klug and Alexander (2) and by Clark (1).
Jean M. Ohrt and Dorita A. Norton, "X-Ray Diffraction Powder Data for Some 5α-Pregnanes," Appl. Spectrosc. 18, 110-112 (1964)