A method to characterize iron oxide microparticles by microquantity X-ray powder diffraction is presented. The method employs small sections of acrylic tubing and double sided Mylar® tape that fits over a standard 170 mm collimator for a Bruker-AXS SMART 1000 or APEXII three-circle single-crystal diffractometer (Mo X-ray tube). The tubing will hold and position a sample that is placed on the double-sided Mylar® tape and allow for rapid specimen mounting/dismounting and data collection. The method is simple, portable, and readily adapted to a variety of single-crystal X-ray diffractometers.