Powder X-ray diffraction sample holder

A method for testing a sample, comprising the steps of:

• (a) fabricating a quartz body having substantially planar top and bottom surfaces that are parallel with each other, the quartz body including a matrix of cylindrical apertures that are substantially perpendicular to the top and bottom surfaces, each aperture in the matrix having an upper opening at the top surface of the quartz body and a lower opening at the bottom surface of the quartz body;
• (b) fusing a quartz bottom sheet to the bottom surface of the quartz body, the quartz bottom sheet including respective portions that close the lower openings of the apertures in the quartz body, such that each aperture and a respective portion of the bottom sheet together form a well for receiving a sample, each aperture and respective portion of the bottom sheet being suitably dimensioned to perform a powder X-ray diffraction technique on a sample contained in the well;
• (c) loading a sample into at least one well in the matrix of wells;
• and
• (d) performing a powder X-ray diffraction technique on the sample.

A method for preparing powder samples from a slurry, comprising the steps of:

• (a) adding a sample of an active pharmaceutical ingredient, counter ions, and solvent to a well in a sample plate formed from a quartz body and a quartz bottom sheet fused thereto, the well and bottom sheet being suitably dimensioned to perform a powder X-ray diffraction technique on a sample contained in the well;
• (b) allowing the sample to age, thereby allowing a slurry to be generated;
• (c) taking a microscopic image of the plate;
• (d) removing remaining solvent;
• (e) taking Raman spectra to determine whether remaining solids contain potentially different forms of active pharmaceutical ingredient;
• and
• (f) using powder X-ray diffraction to further confirm the remaining solids.