Ultra-low oxygen, liquid sample cell for in situ synchrotron-based small-wide angle scattering (SAXS-WAXS)

DOI: 10.1063/5.0146013

Authors: M. Hassan Sk (University of Cambridge) , S. Agrawal (University of Cambridge) , M. Woolley (University of Cambridge) , S. M. Clarke (University of Cambridge) , A. Osundare (The University of Manchester) , D. Craske (The University of Manchester) , Robert Lindsay (The University of Manchester) , Andrew J. Smith (The University of Manchester) , T. Snow (Diamond Light Source) , T. Zinn (Diamond Light Source) , N. Terrill (Diamond Light Source)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Review Of Scientific Instruments , VOL 94

State: Published (Approved)
Published: April 2023
Diamond Proposal Number(s): 23699 , 28693 , 32669

Abstract: Here, we report the design and successful implementation of an ultra-low oxygen sample cell for use on the SAXS-WAXS (small-wide angle x-ray scattering) beamline I22 at DIAMOND. The rigorous exclusion of oxygen is found to require double jacketing with purge gas throughout the entire system, pipework, pumps, and the sample cell itself. This particularly includes a “double-window” arrangement at the sample location to accommodate the very tight geometrical restrictions of the sample position. The in situ cell design also requires the additional complexity of heating the sample/solution and real-time electrochemical measurements. We demonstrate the successful implementation of this arrangement with real-time in situ characterization of an iron foil corrosion evolving under the “sweet-scale environment,” very anoxic conditions common, in particular, commercial situations. The formation of iron carbonate, siderite, rather than iron oxide, indicates that our system is oxygen free down very low levels (<35 ppb at 80 °C).

Journal Keywords: X-ray scattering; X-ray diffraction; In situ small angle X-ray scattering spectroscopy; Synchrotrons; Corrosion

Subject Areas: Technique Development, Materials, Chemistry


Instruments: I22-Small angle scattering & Diffraction

Added On: 12/04/2023 08:36

Discipline Tags:

Technique Development - Materials Science Physical Chemistry Chemistry Corrosion Materials Science

Technical Tags:

Scattering Small Angle X-ray Scattering (SAXS)