Silver behenate, a possible low‐angle diffraction standard, was characterized using the powder diffraction technique. Diffraction patterns obtained with 1.54 Å synchrotron and Cu Kα radiations showed thirteen regularly spaced (00l) peaks in the range 1.5–20.0°2θ. With the National Institute of Standards and Technology's standard reference material silicon as an internal standard, the long spacing of silver behenate was accurately determined from the profile‐fitted synchrotron diffraction peaks, with d001 = 58.380 (3) Å. This result was in agreement with that obtained from the Cu Kα pattern. The profile widths of the silver behenate peaks were found to be consistently larger than those of the silicon peaks, indicating significant line broadening for silver behenate. The average crystallite size along the long‐spacing direction of silver behenate was estimated using the Scherrer equation, giving Davg = 900 (50) Å. Because silver behenate has a large number of well defined diffraction peaks distributed evenly in the 1.5–20.0°2θ range, it is suitable for use as an angle‐calibration standard for low‐angle diffraction. However, care must be taken if silver behenate is to be used as a peak‐profile calibration standard because of line broadening.

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A task group of the JCPDS-International Center for Diffraction Data (ICDD) was established with the charge of investigating the use of silver behenate, CH 3 (CH 2 ) 2 oCOO-Ag, as a possible low-angle calibration standard for powder diffraction applications. Utilizing several data collection and analysis techniques, long-period spacing (JQOI) values with a range of 58.219-58.480 A were obtained. Using the same collected data and one data analysis refinement calculation method resulted in d m values with a range of 58.303-58.425 A. Data collected using a silicon internal standard and the same singular data analysis calculation method provided d^ values with a range of 58.363-58.381 A.

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