Synchrotron X-ray Diffraction for Early Characterisation of Sealed Mars2020 Samples
Authors: Adam Lukas , Bridges John , Bowden Donald , Holt John , Bedford Candice 
Published: February 2023

NASA, ESA and the UK are collaborating on a Mars Sample Return (MSR) mission which aims to retrieve drill cores of Martian rock for terrestrial analysis, starting with the Mars2020 rover which landed successfully in Jezero Crater in Feb. 2021. Up to 30 samples, inside sealed titanium sample tubes, are planned to be returned to Earth in later missions. Due to the potential for back-contamination of Earth from possible extant life on Mars, strict contamination control measures must be taken for the purposes of planetary protection, as well as to prevent contamination of the samples by Earth&#8217;s environment. These measures place restrictions on the way measurements can be performed on the samples until they have been sterilised or judged safe. As the first step of scientific analysis, all samples will undergo a set of measurements called Pre-Basic Characterisation. Pre-BC will include weighing, X-ray CT, and magnetic measurements. These data along with Basic Characterisation data will be used to decide experimental plans for multi instrument analyses on the Mars samples. X-ray Diffraction (XRD) is currently planned for a later stage of sample analysis after the sample tubes have been opened due to limitations with conventional commercial X-ray diffractometers. [1, 2]While a conventional X-ray tube cannot provide an appropriate X-ray beam, a synchrotron source is capable of much higher intensities and precise wavelength selectivity. Synchrotron facilities also allow more suitable diffraction geometries for the size and shape of sample expected from MSR. We have carried out experiments with the help of Diamond Light Source&#8217;s I12-JEEP beamline to test the feasibility of XRD analysis of samples in sealed Mars2020 sample tubes and suitable instrument parameters for XRD of these samples. Titanium tubes were prepared as analogues to Mars2020 sample tubes. Three different geological analogues were used in place of the Mars samples: an Icelandic basaltic sand, a calcareous mudstone from Watchet Bay, UK, and a Devonian Fine Grained Sandstone, UK. Two different methods for preventing unwanted diffraction signal from the sample tube walls have also been tested: subtracting the diffraction spectrum of an empty tube from the tube-with-sample spectrum, and using energy-dispersive X-ray diffraction to exclude tube wall signal. We show that quantitative XRD phase analysis can be successfully carried out on returned Mars samples in unopened sample tubes using a synchrotron X-ray source, and thus could be included in the Pre-BC phase of returned sample science. This would provide mineralogical data much earlier in the sample science process, improving decision-making around sample science, curation, and handling.&#160;References:1.&#160; &#160; &#160; &#160;Meyer, M.A., et al., Final Report of the Mars Sample Return Science Planning Group 2 (MSPG2). Astrobiology, 2022. 22(S1): p. S-5-S-26.2.&#160; &#160; &#160; &#160;Tait, K.T., et al., Preliminary Planning for Mars Sample Return (MSR) Curation Activities in a Sample Receiving Facility (SRF). Astrobiology, 2022. 22(S1): p. S-57-S-80.