Containment of fluid samples in the hydrothermal diamond-anvil cell without the use of metal gaskets: Performance and advantages for in situ analysis

Metal gaskets (Re, Ir, Inconel, or stainless steel) normally used to contain fluid samples in the hydrothermal diamond-anvil cell (HDAC) are sometimes undesirable due to possible contamination and to gasket deformation at high pressures and temperatures resulting in nonisochoric behavior. Furthermore, in x-ray spectroscopic experiments, metal gaskets may attenuate the incident x-ray beam and emitted fluorescence x-rays, and the interaction of scattered radiation with the gasket may produce fluorescence that interferes with the x-ray spectrum of the sample. New arrangements and procedures were tested for the operation of the HDAC without using the metal gaskets. Distilled, de-ionized water was loaded into the sample chamber, a laser-milled recess 300 mu m in diameter and similar to 50 mu m deep centered in the 1.0 mm face of the lower diamond anvil, and sealed by pressing the top diamond anvil face directly against the lower one without a metal gasket in between. A maximum sample pressure of 202 MPa at 617 degrees C was maintained for a duration of 10 min without evidence of leakage. A small change in fluid density was observed in one experiment where the sample was held at 266 MPa at 708 degrees C for 10 min. The gasketless HDAC was also employed in x-ray absorption spectroscopy experiments, where, in addition to the sample chamber in the lower diamond, two grooves were milled at a 90 degrees angle to each other around the sample chamber to minimize the attenuation of incident and fluorescent x rays. With a minimum distance between the sample chamber and the grooves of 80 mu m, a pressure of 76 MPa at 500 degrees C was maintained for 2 h with no change in the original fluid density.