PMID- 19045909 OWN - NLM STAT- MEDLINE DCOM- 20090212 LR - 20131121 IS - 1089-7623 (Electronic) IS - 0034-6748 (Linking) VI - 79 IP - 11 DP - 2008 Nov TI - Containment of fluid samples in the hydrothermal diamond-anvil cell without the use of metal gaskets: performance and advantages for in situ analysis. PG - 115103 LID - 10.1063/1.3013788 [doi] AB - 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 microm in diameter and approximately 50 microm 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 microm, a pressure of 76 MPa at 500 degrees C was maintained for 2 h with no change in the original fluid density. FAU - Chou, I-Ming AU - Chou IM AD - National Center, U.S. Geological Survey, Reston, Virginia 20192, USA. imchou@usgs.gov FAU - Bassett, William A AU - Bassett WA FAU - Anderson, Alan J AU - Anderson AJ FAU - Mayanovic, Robert A AU - Mayanovic RA FAU - Shang, Linbo AU - Shang L LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PT - Research Support, U.S. Gov't, Non-P.H.S. PL - United States TA - Rev Sci Instrum JT - The Review of scientific instruments JID - 0405571 RN - 059QF0KO0R (Water) RN - 7782-40-3 (Diamond) SB - IM MH - Absorptiometry, Photon MH - Atmospheric Pressure MH - Diamond/*chemistry MH - Equipment Design MH - Specimen Handling/*instrumentation MH - Temperature MH - Time Factors MH - Water/chemistry EDAT- 2008/12/03 09:00 MHDA- 2009/02/13 09:00 CRDT- 2008/12/03 09:00 PHST- 2008/12/03 09:00 [pubmed] PHST- 2009/02/13 09:00 [medline] PHST- 2008/12/03 09:00 [entrez] AID - 10.1063/1.3013788 [doi] PST - ppublish SO - Rev Sci Instrum. 2008 Nov;79(11):115103. doi: 10.1063/1.3013788.