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Ultra-low oxygen, liquid sample cell for in situ synchrotron-based small-wide angle scattering (SAXS-WAXS)
M Hassan Sk1,2, S Agrawal1, M Woolley1
1Yusuf Hamied Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, United Kingdom.
The Review of Scientific Instruments
|December 11, 2023
Summary
Researchers developed an ultra-low oxygen sample cell for X-ray scattering studies. This new system successfully characterized iron corrosion under anoxic conditions, forming iron carbonate instead of iron oxide.
Area of Science:
- Materials Science
- Analytical Chemistry
- Corrosion Science
Background:
- Characterizing materials under anoxic conditions is crucial for understanding various industrial processes.
- Existing techniques often struggle to maintain the extremely low oxygen levels required for sensitive experiments.
Purpose of the Study:
- To design and implement an ultra-low oxygen sample cell for in situ small- and wide-angle X-ray scattering (SAXS-WAXS) studies.
- To demonstrate the cell's capability in characterizing corrosion under highly anoxic "sweet-scale" environments.
Main Methods:
- Development of a double-jacketed sample cell with continuous purge gas flow.
- Incorporation of a "double-window" arrangement for X-ray access within tight geometrical constraints.
- Integration of sample heating and real-time electrochemical measurements.
Main Results:
- Successful implementation of the ultra-low oxygen sample cell at the SAXS-WAXS beamline I22.
- Real-time in situ characterization of iron foil corrosion under anoxic conditions (<35 ppb oxygen at 80°C).
- Observation of siderite (iron carbonate) formation, confirming the absence of oxygen and preventing iron oxide formation.
Conclusions:
- The developed ultra-low oxygen sample cell is effective for in situ SAXS-WAXS analysis under stringent anoxic conditions.
- The system enables the study of corrosion mechanisms in environments relevant to commercial applications.
- This technology advances the capability to investigate material behavior in oxygen-depleted settings.
