The authors would like to gratefully acknowledge two anonymous peer reviewers and JoVE senior review editor Dr. Alisha DSouza for their invaluable comments. This research was performed at 6-BM-B of the Advanced Photon Source (APS) at Argonne National Laboratory. The use of this facility has been supported by Consortium for Materials Properties Research in Earth Sciences (COMPRES) under National Science Foundation (NSF) cooperative agreement EAR 11-57758, EAR 1661511 and by the Mineral Physics Institute, Stony Brook University. The authors acknowledge NSF for research funding for this program through EAR 1361463, EAR 1045629, and EAR 1141895. This research used resources of the Advanced Photon Source, a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under contract DEAC02-06CH11357. The cell assemblies are under COMPRES multi-anvil cell assembly development project. All the data files are available from the authors upon request (scheung9@wisc.edu). The samples and data are archived at Mineral Physics Institute at Stony Brook University.

1. Sample Preparation
<ol>
	<li>Choose the test and/or reference sample; this can be either a rock core (step 1.2) or a mineral aggregate (step 1.3), depending the focus of the experimental study. 
	NOTE: The following method is certainly not the only way to prepare good quality samples (e.g., other machines can be used). However, the sample preparation adopted in the present study is fully illustrated to achieve the goal of accurate replication.</li>
	<li>Rock core samples
	<ol>
		<li>Saw a small rectangular slab from a larger sample rock block. Then surface grind the sample slab such that all six surfaces of the slab are flat and perpendicular to their adjacent surfaces.</li>
		<li>To minimize any movement of the sample slab during core drilling, start by placing a machine vice (Figure 2a) on a working surface that is highly stable. Ensure that all contact surfaces are clean so that non-perpendicularity is not introduced to the setup. Place the sample slab between the vice jaws (Figure 2a) and screw the jaws together ensuring that they are just tight enough to secure the sample without damaging it.</li>
		<li>Setup a rotatory tool with a rotatory workstation package as a coring drill press (Figure 2a). Insert a 2 mm (inner diameter) coring diamond drill bit into an adjustable chuck of the drill press. Screw and lock the core drill bit to ensure the assembly is stable during drilling.</li>
		<li>Turn on the rotatory tool and start lowering the drill assembly towards the sample slab. 
		NOTE: Heat is produced at the drill bit tip as the drilling progresses. Excess heat could cause the diamonds at the drill bit tip to wear at an accelerated rate. Since the rotatory drill press is not equipped with a water cooling system, and since our sample size is in the millimeter range, the drill bit can be cooled by injecting coolant manually onto the contact between the rotating drill bit and the slab.</li>
		<li>Drill to the depth of at least 3.25 mm (double of the ideal final height of the sample) so that substantial height is left for end surface preparation afterwards.
		<ol>
			<li>If after retracting the drill bit, the drilled core is still attached to the sample slab, then insert the drill bit around the core and wiggle it slowly until the core is detached from the slab.</li>
			<li>If the drilled core is already detached and stuck in the interior of the core drill bit, then insert a pin of diameter 1.85 mm from the opposite end to push the core towards the outside for retrieval.</li>
		</ol>
		</li>
		<li>Use wipes to dry the cooling water, and then air dry the retrieved samples for at least 2 h or, if possible, overnight. Clean the ground dust around the core by rolling it on a piece of low adhesive tape. Measure the diameter of the core and prioritize the samples by a diameter closest to 1.9+ mm.</li>
		<li>Next prepare for surface grinding of the end surfaces. 
		NOTE: It is extremely important to have the end surface contacts flat so that the applied load can be evenly distributed across the entire surface area.
		<ol>
			<li>Place sand paper under the grinding jig (Figure 2b). Start grinding with coarse grit (e.g., 600 grit), progress towards a finer grit, and finish with at least a 1,500 grit. Insert the core into one end of the hole of the grinding jig. Place tape around the core if it does not fit tightly into the hole of the jig. 
			NOTE: Ensure the work surface remains clean to ensure perpendicularity.</li>
			<li>Insert a pin (diameter of 1.4 mm) into the other end of the hole. Keep holding the pin gently downwards to keep the sand paper and core in contact (Figure 2b). Maintain this position and start slowly grinding the core against the sand paper. Take the core out of the jig and check often to see if the final height (1.67 mm) is reached and if the surface is even.</li>
			<li>For parallelism, insert the sample back to the jig for further grinding, until it reaches a precision within 0.5&#176;.</li>
		</ol>
		</li>
		<li>To assist in deciding on which sample is the best to use, check the overall shape of the samples using a low magnification (2X&#8211;8X) microscope. If possible, obtain some microscopic photographs of the samples for documentation as well.</li>
	</ol>
	</li>
	<li>Mineral aggregate samples
	<ol>
		<li>Prepare mineral grains by first grinding a suitably sized sample of rock or pre-existing powder in a pestle and mortar. 
		NOTE: This process can be sped up by using a rotatory tool with a grinding head, instead of the pestle.</li>
		<li>Use a low magnification microscope to measure the grain size. Continue grinding until the average diameter of the grains is 4 &#181;m.
		<ol>
			<li>Suspend the grains in ethanol. Then separate the grains from the ethanol suspension by using a tall decantation column (~20 cm in height) and settling by gravity. 
			NOTE: The removal of grains that are smaller and larger than 4 &#181;m (&#177; 0.5 &#181;m), is based on their mass. The gravitational force acting on the grain is given by: 
			<img alt="Equation 1" src="/files/ftp_upload/57555/57555eq1.jpg" /> 
			where m is the mass, and g is the acceleration due to gravity. The forces opposing the motion are buoyancy and drag force. The buoyancy force is given by Archimedes&#8217; principal: 
			<img alt="Equation 3" src="/files/ftp_upload/57555/57555eq3.jpg" /> 
			where &#961; is the density, and V is the volume of the displaced fluid. The drag force is given by: 
			<img alt="Equation 4" src="/files/ftp_upload/57555/57555eq4.jpg" /> 
			where u is the particle-fluid relative velocity, Ap is the area of the particle projected in direction of the motion, and CD is the drag coefficient. By balancing the forces, set the boundary condition at which the grains reach the terminal velocity. Assuming laminar flow conditions, the velocity of the grain vgrain is given in the resulting equation known as Stokes&#8217; Law: 
			<img alt="Equation 5" src="/files/ftp_upload/57555/57555eq5.jpg" /> 
			where d is the diameter of the grain.</li>
		</ol>
		</li>
		<li>Extract the ethanol/grain mix at different heights in the column into separate glass beakers, to obtain grains sorted by their grain diameter. 
		NOTE: The rate of grain settling depends on its diameter and density.</li>
		<li>Leave the content in the beakers overnight to air dry. Measure the final average diameter of the grains using a low magnification microscope and select the batch of grains with a diameter closest to 4 &#181;m (for optimal X-ray signals).</li>
	</ol>
	</li>
</ol>
2. Cell Assembly Preparation
<ol>
	<li>Load the prepared samples into a standard D-DIA cell assembly (Figure 3a). 
	NOTE: The D-DIA cell assembly was developed under the Consortium for Materials Properties Research in Earth Sciences (COMPRES) multi-anvil cell assembly development project14. The following description of the standard D-DIA cell design (under the COMPRES project) can be used for an addition of increased temperature if desired.
	<ol>
		<li>Start with a cell assembly cube (6.18 mm edge length; Figure 3) on a clean working surface.</li>
		<li>Clean an alumina rod (diameter of 1.5 mm, height of 1.46 mm; Figure 3a), an alumina ring (Figure 3a), and a graphite ring (Figure 3a) in an ultrasonic bath. Prepare the end surfaces of the alumina rod flat and parallel to a precision within 0.5&#176; (refer to Section 1.2.7).</li>
		<li>Put a piece of tape at one end of the hole of the cube. Use a pair of tweezers to put the two rings around the alumina rod, and insert them all the way down into the hole of the cube, and such that the graphite ring is in contact with the tape. 
		NOTE: The alumina ring is used as a separator; the graphite ring is used for electrical conductivity upon higher temperature application (not applied for the cold compression presented in this study).</li>
		<li>Mark the corner of the cube to be aligned with the incoming X-ray beam direction (Figure 4b). 
		NOTE: The tantalum foil is used to obtain better contrast for quantifying the sample volume using radiography during the experiment (Section 3).
		<ol>
			<li>Cut a rectangular piece of tantalum foil (1.5 mm x 17 mm). Fold the foil into a U-shape piece (see Figure 3b for more details) and place inside the cylindrical space of the cell assembly. To ensure a tight fit between the foil and the edges of the cylindrical space, use a pin (diameter of 1.83 mm) to push onto the foil against the edges to remove any excess space between the two.</li>
			<li>Align this U-shaped foil with respect to the X-ray beam direction (Figure 4a), and aim to minimize and maximize the 2-D projection of the foil and the samples, respectively.</li>
		</ol>
		</li>
		<li>Lay a piece of rectangular tantalum foil (1.7 mm x 1 mm) on top of the rock core (Figure 3b). Make sure the foil is flat, and align the foil such that the length (1.7 mm) of the foil is perpendicular to the X-ray beam direction (Figure 4a). 
		NOTE: Either a rock core or mineral aggregate can be a &#8220;reference sample&#8221;, depending on the goal of the experimental study. In this particular example, insert the rock core prepared in Section 1.2. as the &#8220;reference sample&#8221; portion in Figure 3b. The purpose of this piece of foil is to provide better contrast of the boundary between adjacent samples.</li>
		<li>Carefully pack the mineral aggregate (prepared in Section 1.3) into the cylindrical space with a spatula (the &#8220;sample&#8221; portion in Figure 3b). 
		NOTE: Again, either a rock core or mineral aggregate can be a &#8220;sample&#8221;, depending on the goal of the experimental study.</li>
		<li>Remove the excess grains adhered to the lateral side of the cylindrical space gently with air if necessary. Use a pin (diameter of 1.83 mm) and a caliper to check if the final height has been reached; leave 1.4 mm in the height for inserting the top alumina rod.</li>
		<li>Insert another rectangular piece of tantalum foil (1.7 mm x 1 mm). Clean a new set of an alumina rod (diameter of 1.5 mm, height of 1.46 mm), an alumina ring, and a graphite ring (Figure 3a) in the ultrasonic bath. Use a pair of tweezers to put the two rings around the alumina rod, and insert them such that remaining space of the cylindrical volume is fully filled with the graphite ring on top.</li>
		<li>Use a minimal amount of cement (zirconium powder mixed with activator) to seal the alumina rod exposed on both ends of the cube. After the cement is dried, trim the excess tantalum foil that is still exposed outside of the cube for tidiness.</li>
	</ol>
	</li>
</ol>
3. Experimental Procedure
NOTE: The following experiment is performed at beamline 6-BM-B (Figure 4a) of the APS at Argonne National Laboratory. The experiment performed at 6-BM-B is under white X-ray mode. This beamline is an open beamline and welcomes proposals from scientists, researchers, and students worldwide to perform experiments under its general user program.
<ol>
	<li>Perform the energy calibration of the system by collecting a diffraction pattern for an alumina standard.
	<ol>
		<li>Collect a diffraction pattern by clicking the &#34;start&#34; button on the &#34;12 Element Detector Control Pump&#34; panel.</li>
		<li>Analyze the alumina XRD pattern, which contains built-in Cobalt-57 (Co-57) fluorescence peaks, by calculating the average peak position (Horiz X, Vert Y, and Beam Z dimensions) over the different detectors.</li>
		<li>Enter the average values as new pedestal positions in the &#34;6motors.adl&#34; panel. Recollect a diffraction pattern and save as an energy dispersive diffraction file (EDF), which constrains the 2-theta angle and the correlation function between the detector channel and X-ray energy for each of the 10 detectors.</li>
	</ol>
	</li>
	<li>Remove the alumina standard and collect an open press X-ray spectrum by clicking the &#34;start&#34; button on the &#34;12 Element Detector Control Pump&#34; panel (with an exposure time of 500 s, to optimize signal-to-noise ratio) to measure the diffraction of the background without any sample assembly.</li>
	<li>Clean the anvils (truncation edge length of 4 mm) with acetone and use a portable vacuum cleaner to remove all debris from previous experiments. Insert the sample assembly prepared in Section 2 into the center of the experiment setup that consists of four, X-ray transparent, sintered diamond and two tungsten carbide (top/bottom) anvils (Figure 4b).</li>
	<li>Slowly lower the opposing pairs of lateral anvils simultaneously. Use a level to check if the anvils are leveled. Gently push the anvil to adjust the alignment until it is all leveled. The bottom and four lateral anvils should now all be in contact with the sample assembly. Release the safety latch and insert the spacer (Figure 4a).</li>
	<li>Close the hutch and enable the shutter to allow the X-ray beam to enter the hutch.</li>
	<li>In the &#34;low-pressure pump panel&#34; (labeled as the pump motor controller module in Figure 5), turn the &#34;low-pressure pump&#34; button ON and push the &#34;up&#34; button next to the &#34;top ram&#34; label to move the top ram to the top, against the spacer (Figure 4a). With the aid of real-time X-radiographic imaging (Figure 5), start moving the bottom ram up slowly and carefully until the anvils start to appear in the radiograph. &#34;Leave a very fine gap&#34; such that the sample is not overloaded initially before the experiment.</li>
	<li>Turn off all the controls on the low-pressure pump controller module (Figure 5) and close the &#8220;pressurize&#8221; valve before starting to compress with the high-pressure hydraulic pump. 
	NOTE: The high-pressure pump is controlled using EPICS-based software (Figure 5). EPICS is a non-commercial set of open source software tools, libraries, and applications developed by Argonne National Laboratory.
	<ol>
		<li>Move the sample position in the Z direction (parallel to the beam) using the &#34;jog&#34; button in the &#34;6motors.adl&#34; panel such that the center of the sample in the ImageJ EPICS area detector plugin software panel aligns with the diffraction focus mark on the screen. This minimizes parasitic diffraction and optimizes the signal-to-noise ratio.</li>
	</ol>
	</li>
	<li>Collect diffraction spectra by clicking the &#34;start&#34; button on the &#34;12 Element Detector Control Pump&#34; panel for the core and the aggregate (&#34;jog&#34; button along pedestal Z to move between samples) separately, each with an exposure time of 500 s, at ambient conditions. On the &#34;NDFileTIFF.adl&#34; panel, click the &#34;capture-start&#34; button to capture a radiograph (Figure 5) of these samples with an exposure time of ~6 ms.</li>
	<li>Drive the anvils inwards by wedged guide blocks running on the hydraulics pump by starting the motor. In the &#34;SAM-85 Press Load Control&#34; window (Figure 6), set the target load to 50 tons. Turn the feedback on, with the upper limit of the speed control set to 7 (the slowest compression possible). 
	NOTE: The press load and speed can be changed depending on the target pressure and the speed of the compression. The maximum press load to avoid the breakage of anvils is 100 tons.</li>
	<li>Use the &#34;Diffraction-Imaging-Scan-Prosilica&#34; panel (Figure 7) to set up an automatic data collection by defining the desired locations of the core (e.g., Press X = 20.738 mm, Press Y = 4.3 mm) and the aggregate (e.g., Press X = 20.738 mm, Press Y = 4.8 mm) for diffraction (with preset exposure times of 500 s) and X-radiographic imaging. Set the cycles required to 0 such that this data collection will repeat continuously. Click &#34;start&#34; to start the data collection. 
	NOTE: As the compression progresses, the sample will move upwards, so new desired locations should be updated accordingly.</li>
	<li>After reaching the target load of 50 ton, click the stop button to stop the automatic data collection in the &#34;Diffraction-Imaging-Scan-Prosilica&#34; panel (Figure 7). In the &#34;SAM-85 Press Load Control&#34; window, decompress the sample by setting the lower limit of the speed control to -10 and change the target load to 0 ton.</li>
	<li>After unloading, collect the diffraction spectra for the core and the aggregate separately, by clicking the &#34;start&#34; button on the &#34;12 Element Detector Control Pump&#34; panel; use an exposure time of 500 s for both the core and the aggregate. On the &#34;NDFileTIFF.adl&#34; panel, click the &#34;capture-start&#34; button to capture a radiograph (Figure 5) of these samples with an exposure time of ~6 ms.</li>
	<li>In the low-pressure pump panel (labeled as the pump motor controller module in Figure 5), open the &#34;pressurize valve&#34;. Push the &#34;low-pressure pump &#8211; on&#34; button. Press the &#34;down&#34; buttons both next to the &#34;top ram&#34; and &#34;bottom ram&#34; labels to move both the top and the bottom ram downwards until the green &#34;Down&#34; light becomes illuminated, then stop driving both rams.</li>
	<li>In the &#34;low-pressure pump&#34; panel, press the out button near the &#34;spacer block&#34; label to move the spacer arm to the &#34;out&#34; position, and then press the &#34;up&#34; button near the &#34;top ram&#34; label to drive the top ram up until the safety lock engages. Turn all the controls off in the pump motor controller unit (Figure 5) afterwards. Slowly and manually move the lateral anvils outwards and remove the sample assembly.</li>
</ol>

<ol><li>Bjørlykke, K. <a target="_blank" href="https://www-sciencedirect-com.bdigitaluss.remotexs.co/science/article/pii/S0037073813002200">Relationships between depositional environments, burial history and rock properties. Some principal aspects of diagenetic processes in sedimentary basins.</a> Sedimentary Geology. , 1-14 (2014).</li>
<li>Burnley, P. C., Zhang, D. <a target="_blank" href="http://iopscience.iop.org/article/10.1088/0953-8984/20/28/285201/meta">Interpreting in situ X-ray diffraction data from high pressure deformation experiments using elastic-plastic self-consistent models: An experiment using quartz.</a> J. Phys. Condens. Matter Solid Earth. 20 (28), 285201(2008).</li>
<li>Burnley, P. C. <a target="_blank" href="https://pubs.geoscienceworld.org/msa/ammin/article/100/7/1424/40502/elastic-plastic-self-consistent-epsc-modeling-of">Elastic plastic self-consistent (EPSC) modeling of plastic deformation of fayalite olivine.</a> American Mineralogist. 100 (7), 1424-1433 (2015).</li>
<li>Chen, J., Li, L., Weidner, D. J., Vaughan, M. T. <a target="_blank" href="https://www-sciencedirect-com.bdigitaluss.remotexs.co/science/article/pii/S0031920104000676">Deformation experiments using synchrotron X-rays: in situ stress and strain measurements at high pressure and temperature.</a> Phys. of the Earth and Planetary Interiors. 143, 347-356 (2004).</li>
<li>Cheung, S. N. C. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=%22Experimental+deformation+in+sandstone%2C+carbonates%2C+and+quartz+aggregate%22">Experimental deformation in sandstone, carbonates, and quartz aggregate</a>. , State University of New York at Stony. Ph.D. Thesis (2015).</li>
<li>Cheung, S. N. C., et al. <a target="_blank" href="http://onlinelibrary.wiley.com/doi/10.1002/2016JB013653/full">Stress distribution during cold compression of a quartz aggregate using synchrotron X-ray diffraction: observed yielding, damage, and grain crushing.</a> J. Geophys. Res. Solid Earth. 122, 2724-2735 (2017).</li>
<li>Croizé, D., Ehrenberg, S. N., Bjørlykke, K., Renard, F., Jahren, J. <a target="_blank" href="https://www-sciencedirect-com.bdigitaluss.remotexs.co/science/article/pii/S0264817209002116">Petrophysical properties of bioclastic platform carbonates: implications for porosity controls during burial.</a> Marine and Petroleum Geology. 27 (8), 1765-1774 (2010).</li>
<li>Doornhof, D., Kristiansen, T. G., Nagel, N. B., Pattillo, P. D., Sayers, C. <a target="_blank" href="https://pdfs.semanticscholar.org/40e4/33ecc9d15e0d01bd77dc8606a93aed0e2564.pdf">Compaction and subsidence.</a> Oilfield rev. 18 (3), 50-68 (2006).</li>
<li>Durham, W. B., Weidner, D. J., Karato, S. <a target="_blank" href="https://pubs.geoscienceworld.org/msa/rimg/article-abstract/51/1/21/87434/new-developments-in-deformation-experiments-at">New developments in deformation experiments at high pressure.</a> Rev. Mineral. Geochem. 51 (1), 22-49 (2002).</li>
<li>Fyfe, W. S. <a target="_blank" href="https://www-sciencedirect-com.bdigitaluss.remotexs.co/science/article/pii/0009254178900682">The evolution of the Earth's crust: modern plate tectonics to ancient hot spot tectonics.</a> Chemical Geology. (1-4), 89-114 (1978).</li>
<li>Gerward, L., Mo, S., Topso, H. <a target="_blank" href="http://aip.scitation.org/doi/abs/10.1063/1.322714">Particle size and strain broadening in energy-dispersive -ray powder patters.</a> J. Appl. Phys. 47 (3), 822-825 (1976).</li>
<li>Heap, M. J., Farquharson, J. I., Baud, P., Lavallée, Y., Reuschlé, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Fracture+and+compaction+of+andesite+in+a+volcanic+edifice%5BTitle%5D)+AND+%22Bulletin+of+volcanology%22%5BJournal%5D)">Fracture and compaction of andesite in a volcanic edifice.</a> Bulletin of volcanology. 77 (6), 55(2015).</li>
<li>Lavina, B., Dera, P., Downs, R. T. <a target="_blank" href="https://pdfs.semanticscholar.org/110f/462d8b072458d713959665e778409e4dff3f.pdf">Modern X-ray diffraction methods in mineralogy and geosci.</a> Reviews in Mineralogy and Geochemistry. 78 (1), 1-31 (2014).</li>
<li>Leinenweber, K. D., et al. <a target="_blank" href="https://pubs.geoscienceworld.org/msa/ammin/article-abstract/97/2-3/353/45562/cell-assemblies-for-reproducible-multi-anvil">Cell assemblies for reproducible multi-anvil experiments (the COMPRES assemblies).</a> American Mineralogist. 97 (2-3), 353-368 (2012).</li>
<li>Li, L., Weidner, D. J., Raterron, P., Chen, J., Vaughan, M. T. <a target="_blank" href="https://www-sciencedirect-com.bdigitaluss.remotexs.co/science/article/pii/S0031920104000688">Stress measurements of deforming olivine at high pressure.</a> Phys. of the Earth and Planetary Interiors. 143, 357-367 (2004).</li>
<li>Li, L., Weidner, D. J., Chen, J., Vaughan, M. T., Davis, M., Durham, W. B. <a target="_blank" href="http://aip.scitation.org/doi/abs/10.1063/1.1738532">X-ray strain analysis at high pressure: Effect of plastic deformation in MgO.</a> J. App. Phys. 95 (12), 8357-8365 (2004).</li>
<li>Minkoff, S. E., Stone, C. M., Bryant, S., Peszynska, M., Wheeler, M. F. <a target="_blank" href="https://www-sciencedirect-com.bdigitaluss.remotexs.co/science/article/pii/S0920410503000214">Coupled fluid flow and geomechanical deformation modeling.</a> J. Petroleum Sci. and Engineering. 38 (1), 37-56 (2003).</li>
<li>Miyagi, L., et al. <a target="_blank" href="https://utah-pure-elsevier-com.bdigitaluss.remotexs.co/en/publications/deformation-and-texture-development-in-cairo3-post-perovskite-pha">Deformation and texture development in CalrO 3 post-perovskite phase up to 6 GPa and 1300 K.</a> Earth and Planetary. 268 (3), 515-525 (2008).</li>
<li>Morton, R. A., Bernier, J. C., Barras, J. A. <a target="_blank" href="https://pubs.er.usgs.gov/publication/70030503">Evidence of regional subsidence and associated interior wetland loss induced by hydrocarbon production, Gulf Coast region, USA.</a> Environmental Geology. 50 (2), 261(2006).</li>
<li>Nagel, N. B. <a target="_blank" href="https://www-sciencedirect-com.bdigitaluss.remotexs.co/science/article/pii/S1464189501000151">Compaction and subsidence issues within the petroleum industry: From Wilmington to Ekofisk and beyond.</a> Phys. And Chem. of the Earth, Part A: Solid Earth and Geodesy. 26 (1-2), 3-14 (2001).</li>
<li>Nichols, G. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aNichols%2C+G+%22Sedimentology+and+Stratigraphy%22">Sedimentology and Stratigraphy</a>. , John Wiley & Sons. (2009).</li>
<li>Nicolas, A., Fortin, J., Regnet, J. B., Dimanov, A., Guéguen, Y. <a target="_blank" href="https://academic-oup-com.bdigitaluss.remotexs.co/gji/article/206/1/438/2606525">Brittle and semi-brittle behaviours of a carbonate rock: influence of water and temperature.</a> Geophysical Journal International. 206 (1), 438-456 (2016).</li>
<li>Nishiyama, N., Wang, Y., Sanehira, T., Irifune, T., Rivers, M. L. <a target="_blank" href="https://www-tandfonline-com.bdigitaluss.remotexs.co/doi/abs/10.1080/08957950802250607">Development of the multi-anvil assembly 6-6 for DIA and DDIA type high-pressure apparatuses.</a> High Pressure Research. 28 (3), 307-314 (2008).</li>
<li>Nur, A., Walder, J. <a target="_blank" href="https://www.nap.edu/read/1346/chapter/9">Time-dependent hydraulics of the Earth's crust.</a> The role of fluids in crustal processes. , 113-127 (1990).</li>
<li>Paterson, M. S. <a target="_blank" href="http://onlinelibrary.wiley.com/doi/10.1029/GM056p0187/summary">Rock deformation experimentation. The brittle-ductile transition in rocks. The Heard Volume.</a> The American Geophysical Union, Geophys. Monograph. 56, 187-194 (1990).</li>
<li>Peng, S. D. <a target="_blank" href="https://www-sciencedirect-com.bdigitaluss.remotexs.co/science/article/pii/1365160971900098">Stresses within elastic circular cylinders loaded uniaxially and triaxially.</a> Int. J. Rock Mech. Min. Sci. Geomech. Abst. 78 (1), 399-432 (1971).</li>
<li>Raterron, P., Merkel, S., Holyoke, C. W. III <a target="_blank" href="Axial temperature and gradient and stress measurements in the deformation D-DIA cell using alumina pistons ">Axial temperature and gradient and stress measurements in the deformation D-DIA cell using alumina pistons.</a> Rev. of Sci. Instr. 84 (4), 043906(2013).</li>
<li>Raghavan, R., Chin, L. Y. <a target="_blank" href="https://www.onepetro.org/journal-paper/SPE-88870-PA">Productivity changes in reservoirs with stress-dependent permeability.</a> SPE Annual Technical Conference and Exhibition. , Soc. of Petroleum Engineers. (2002).</li>
<li>Reynolds, C. A., Menke, H., Andrew, M., Blunt, M. J., Samuel, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Dynamic+fluid+connectivity+during+steady-state+multiphase+flow+in+a+sandstone%5BTitle%5D)+AND+%22Proceedings+of+National+Academy+of+Sci%22%5BJournal%5D)">Dynamic fluid connectivity during steady-state multiphase flow in a sandstone.</a> Proceedings of National Academy of Sci. 114 (31), 8187-8192 (2017).</li>
<li>Scholle, P. A. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aScholle%2C+PA+%22A+color+illustrated+guide+to+constituents%2C+textures%2C+cements%2C+and+porosities+of+sandstones+and+associated+rocks%22">A color illustrated guide to constituents, textures, cements, and porosities of sandstones and associated rocks</a>. , AAPG Memoir 28 (1979).</li>
<li>Scholle, P. A., Ulmer-Scholle, D. S. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aScholle%2C+PA+%22A+Color+Guide+to+the+Petrography+of+Carbonate+Rocks%3A+Grains%2C+Textures%2C+Porosity%2C+Diagenesis%22">A Color Guide to the Petrography of Carbonate Rocks: Grains, Textures, Porosity, Diagenesis</a>. , AAPG Memoir 77 (2003).</li>
<li>Scholz, C. H. <a target="_blank" href="http://onlinelibrary.wiley.com/doi/10.1029/JB073i004p01447/abstract">Experimental study of the fracturing process in brittle rock.</a> J. Geophys. Res. 73 (4), 1447-1454 (1968).</li>
<li>Schutjens, P. M. T. M., et al. <a target="_blank" href="https://www.onepetro.org/journal-paper/SPE-88441-PA">Compaction-induced porosity/permeability reduction in sandstone reservoirs: Data and model for elasticity-dominated deformation.</a> SPE Reservoir Evaluation & Engineering. 7 (3), 202-216 (2004).</li>
<li>Simmons, G., Wang, H. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aSimmons%2C+G+%22Single+Crystal+Elastic+Constants+and+Calculated+Aggregate+Properties%22">Single Crystal Elastic Constants and Calculated Aggregate Properties</a>. , MIT Press. Cambridge, MA. 135-160 (1971).</li>
<li>Singh, A. K., Balasingh, C., Mao, H. K., Hemley, R. J., Shu, J. <a target="_blank" href="http://aip.scitation.org/doi/abs/10.1063/1.367872">Analysis of lattice strains measured under nonhydrostatic pressure.</a> J. Applied physics. 83 (12), 7567-7575 (1998).</li>
<li>Terzaghi, K. V. <a target="_blank" href="http://www.scirp.org/(S(351jmbntvnsjt1aadkposzje))/reference/ReferencesPapers.aspx?ReferenceID=790257">Die berechnung der durchlassigkeitsziffer des tones aus dem verlauf der hydrodynamischen spanningsercheinungen.</a> Sitzungsberichte der Akademie der Wissenschften in Wein. Mathematisch-Naturwissenschaftliche Klasse. Abteilung lla. 132, 125-138 (1923).</li>
<li>Wang, Y., Durham, W. B., Getting, I. C., Weidner, D. J. <a target="_blank" href="http://aip.scitation.org/doi/abs/10.1063/1.1570948">The deformation D-DIA: a new apparatus for high temperature triaxial deformation to pressures up to 15 GPa.</a> Rev. Sci. Instrum. 74 (6), 3002-3011 (2003).</li>
<li>Wang, Y., Hilairet, N., Dera, P. <a target="_blank" href="https://link-springer-com.bdigitaluss.remotexs.co/article/10.1007/s12583-010-0124-y">Recent advances in high pressure and temperature rheological studies.</a> J. Earth Sci. 21 (5), 495-516 (2010).</li>
<li>Weidner, D. J., et al. <a target="_blank" href="http://onlinelibrary.wiley.com/doi/10.1029/GM067p0013/summary">Characterisation of Stress, Pressure, and Temperature in SAM85, a DIA Type High Pressure Apparatus.</a> Geophys. Monogr. Ser. AGU. , Washington, D.C. 13-17 (1992).</li>
<li>Weidner, D. J., Wang, Y., Vaughan, M. T. <a target="_blank" href="https://www.ncbi.nlm.nih.gov/pubmed/17816686">Strength of diamond.</a> Sci. 266 (5184), 419-422 (1994).</li>
<li>Weidner, D. J. <a target="_blank" href="https://pubs.geoscienceworld.org/msa/rimg/article-abstract/37/1/493/87402/rheological-studies-at-high-pressure">Rheological studies at high pressure.</a> Rev. in Mineralogy and Geochemistry. 37 (1), 493-524 (1998).</li>
<li>Weidner, D. J., Wang, Y., Chen, G., Vaughan, M. T. <a target="_blank" href="http://onlinelibrary.wiley.com/doi/10.1029/GM101p0473/summary">Rheology measurements at high pressure and temperature.</a> Properties of Earth and Planetary Materials at High Pressure and Temperature. AGU. , Washington, D.C. 473-482 (1998).</li>
<li>Weidner, D. J., Vaughan, M. T., Wang, L., Long, H., Li, L., Dixon, N. A., Durham, W. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Precise+stress+measurements+with+white+synchrotron+x+rays%5BTitle%5D)+AND+%22Rev.+of+Sci.+Instrum%22%5BJournal%5D)">Precise stress measurements with white synchrotron x rays.</a> Rev. of Sci. Instrum. 81 (1), 013903(2010).</li>
<li>Weidner, D. J., Li, L., Whitaker, M., Triplett, R. <a target="_blank" href="http://onlinelibrary.wiley.com/doi/10.1002/2017JB014753/abstract">Ultrasonic Acoustic Velocities During Partial Melting of a Mantle Peridotite KLB-1.</a> J. Geophys. Res: Solid Earth. , (2018).</li>
<li>Whitaker, M. L., Baldwin, K. J., Huebsch, W. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((DIASCoPE%3A+Directly+integrated+acoustic+system+combined+with+pressure+experiments-A+new+method+for+fast+acoustic+velocity+measurements+at+high+pressure%5BTitle%5D)+AND+%22Rev.+Sci.+Instrum%22%5BJournal%5D)">DIASCoPE: Directly integrated acoustic system combined with pressure experiments-A new method for fast acoustic velocity measurements at high pressure.</a> Rev. Sci. Instrum. 88 (3), 034901(2017).</li>
</ol>

The authors declare no conflict of interest.

We present the detailed procedure for carrying out XRD experiments using the multi-anvil cell at 6-BM-B. Perhaps the most critical, and yet most challenging, steps in the above protocol involve optimizing the quality of the sample. Such importance on sample quality applies to almost all rock and mineral deformation experiments. Firstly, it is critical for the end surface of the rock cores to be flat, with both ends parallel to each other and at the same time, perpendicular to the cylindrical surface. That will ensure the...

The rationale behind the method presented in this article is to quantify the stress distribution within rock and mineral aggregate samples during compression and subsequent compaction. Understanding the compaction in rocks and mineral aggregates is of great importance to reservoir and geotechnical engineering8,17,18,19,20,28,33. Compaction acts to reduce porosity, and therefore, leads to an increase in pore pressure. Any such increase in pore pressure leads to a decrease in effective pressure35. The consequence is that it will significantly weaken the reservoir rock, and can therefore be subjected to premature failure at lower stress. Some examples of the resulting consequences of inelastic deformation in the subsurface include: failure in sustaining long term production in oil and gas reservoirs28,33, surface subsidence8,18,19,20, and alteration of fluid flow patterns17. Therefore, a comprehensive knowledge of compaction processes in rocks and mineral aggregates could aid in reducing the possibility of such potentially negative consequences.
The great advantage of using the method highlighted here is that it provides a means to quantify stress distribution internally within a geomaterial5,6 with respect to the globally-averaged externally applied pressure12,22. Moreover, as an in situ experiment, the evolution of the stress distribution is time-resolved. The externally applied pressures considered range from relatively low values (tens of megapascals) to high values (several gigapascals). The stress within the sample is measured indirectly by using the atomic lattice spacing within individual mineral grains as a measure of the local elastic strain5,6. The atomic lattice spacing is determined with the aid of X-radiation, commonly in either the mode of white or monochromatic X-ray. For the white X-ray mode (e.g., DDIA at 6BM-B beamline of the Advanced Photon Source (APS), Argonne National Laboratory), the intensity of the diffracted beam X-ray beam is determined by not just one, but by an array of 10-element Ge detectors (Figure 1) distributed along a fixed circle at azimuthal angles of 0&#176;, 22.5&#176;, 45&#176;, 67.5&#176;, 90&#176;, 112.5&#176;, 135&#176;, 157.5&#176;, 180&#176;, 270&#176;. For the monochromatic X-ray mode, the diffracted pattern is recorded using a CCD detector (e.g., DDIA-30 at 13-ID-D beamline of the GSECARS, APS, Argonne National Laboratory)18,23. Both X-ray modes allow quantification on how the stress varies in different orientations. This approach is fundamentally different from all previous studies of compaction in geomaterials.
In typical compaction studies, a cylindrical sample is compressed by an axial force that is applied across the cross-sectional area by the actuator25. Under such conditions, the magnitude of the applied stress magnitude is generally calculated by simply dividing the axial force (measured by a load cell) by the initial cross-sectional area of the sample. It should be noted that this applied stress magnitude is merely an average, bulk value and, as such, does not realistically represent how the local stress state varies, or is distributed, within a complex, heterogeneous, granular material. Detrital sedimentary rocks, which are examples of complex granular materials, are formed by aggregation of mineral grains that are subsequently compacted and cemented through depositional and diagenetic processes1,7,21,30,31. These aggregates naturally inherit pores that comprise the void spaces between grains, which are intrinsic from the geometry of grain packing modified by secondary dissolution. Hence, any applied stress is expected to be supported by and concentrated at grain-to-grain contacts, and to vanish at grain-pore interfaces.
In addition to the complexity of stress variation within a granular material, other factors further complicate studying compaction in these scenarios. First, the local stress field is vulnerable to any changes due to microstructural artifacts (e.g., grain shape, preexisting fractures) that are inevitably present within any detrital sedimentary rock. Second, although the magnitude of the applied stress acting upon the sample surfaces can be fully quantified, the distribution of stresses within the sample body remained poorly constrained. An end effect32 &#8212; a boundary effect whereby the average stress is concentrated near the contact between the loading rams and the samples due to interface friction &#8212; is well known to be exhibited in cylindrical samples loaded in compression. As an example, Peng26 demonstrated strain heterogeneity within uniaxially compressed granite samples subjected to a variety of end conditions. Hence, to accurately compute the local stress distribution in granular material, we present the following detailed protocol for performing X-ray diffraction (XRD) experiments on rocks and mineral aggregates, using a multi-anvil deformation apparatus at beamline 6-BM-B of the APS at Argonne National Laboratory.

<table><tbody><tr><td>Rotatory Tool Workstation Drill Press Work Station with Wrench</td><td>Dremel</td><td>220-01</td><td></td></tr><tr><td>MultiPro Keyless Chuck</td><td>Dremel</td><td>4486</td><td></td></tr><tr><td>Variable-Speed Rotatory Tool&amp;nbsp;</td><td>Dremel</td><td>4000-6/50</td><td></td></tr><tr><td>Super small Diamond Core Drill - 2.5 mm</td><td>Dad&#039;s Rock Shop</td><td>SDCD</td><td></td></tr><tr><td>Coolant</td><td>NBK</td><td>JK-A-NBK-000-020</td><td>Grinding Fluid Concentrate US 5 gal / 20 L</td></tr><tr><td>commercial software package and codes for instrument control and data acquisition</td><td>IDL EPICS and SPEC</td><td></td><td>installed on the computer at the beamline</td></tr><tr><td>CCD Camera</td><td>Allied Vision</td><td>Prosilica GT</td><td>installed at the beamline</td></tr></tbody></table>

stress distribution during cold compression of rocks and mineral aggregates using synchrotron-based x-ray diffraction

We report detailed procedures for performing compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus (D-DIA) coupled with synchrotron X-radiation. A cube-shaped sample assembly is prepared and compressed, at room temperature, by a set of four X-ray transparent sintered diamond anvils and two tungsten carbide anvils, in the lateral and the vertical planes, respectively. All six anvils are housed within a 250-ton hydraulic press and driven inward simultaneously by two wedged guide blocks. A horizontal energy dispersive X-ray beam is projected through and diffracted by the sample assembly. The beam is commonly in the mode of either white or monochromatic X-ray. In the case of white X-ray, the diffracted X-rays are detected by a solid-state detector array that collects the resulting energy dispersive diffraction pattern. In the case of monochromatic X-ray, the diffracted pattern is recorded using a two-dimensional (2-D) detector, such as an imaging plate or a charge-coupled device (CCD) detector. The 2-D diffraction patterns are analyzed to derive lattice spacings. The elastic strains of the sample are derived from the atomic lattice spacing within grains. The stress is then calculated using the predetermined elastic modulus and the elastic strain. Furthermore, the stress distribution in two-dimensions allow for understanding how stress is distributed in different orientations. In addition, a scintillator in the X-ray path yields a visible light image of the sample environment, which allows for the precise measurement of sample length changes during the experiment, yielding a direct measurement of volume strain on the sample. This type of experiment can quantify the stress distribution within geomaterials, which can ultimately shed light on the mechanism responsible for compaction. Such knowledge has the potential to significantly improve our understanding of key processes in rock mechanics, geotechnical engineering, mineral physics, and material science applications where compactive processes are important.

We show one representative result example from an XRD experiment (experiment SIO2_55) run in the multi-anvil press at 6BM-B on a compound quartz aggregate5,6 and novaculite core sample6. The grain sizes of the quartz aggregate and novaculite are ~4 &#181;m and ~6&#8211;9 &#181;m, respectively5,6. Selected diffraction spectra collected during this ex...

Watch this Scientific Journal Video about Stress Distribution During Cold Compression of Rocks and Mineral Aggregates Using Synchrotron-based X-Ray Diffraction at JoVE.com

Stress Distribution During Cold Compression of Rocks and Mineral Aggregates Using Synchrotron-based X-Ray Diffraction

We report detailed procedures for compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus coupled with synchrotron X-radiation. Such experiments allow quantification of the stress distribution within samples, that ultimately sheds light on compaction processes in geomaterials.

We report detailed procedures for performing compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus (D-DIA) ...

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Principal Stresses under a Given Loading

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9.7K Views.  Stony Brook University. Wij rapporteren gedetailleerde procedures voor compressie experimenten over rotsen en minerale aggregaten binnen een multi aambeeld vervorming apparaat synchrotron straling wordt gekoppeld. Dergelijke experimenten kunnen de kwantificering van de stress-distributie binnen monsters, die uiteindelijk licht op verdichting processen in geomaterials werpt.

Video: Stress Distribution During Cold Compression of Rocks and Mineral Aggregates Using Synchrotron-based X-Ray Diffraction

Measuring Fluxes of Mineral Nutrients and Toxicants in Plants with Radioactive Tracers

Unidirectional influx and efflux of nutrients and toxicants, and their resultant net fluxes, are central to the nutrition and toxicology of plants. Radioisotope tracing is a major technique used to measure such fluxes, both within plants, and between plants and their environments. Flux data obtained with radiotracer protocols can help elucidate the capacity, mechanism, regulation, and energetics of transport systems for specific mineral nutrients or toxicants, and can provide insight into compartmentation and turnover rates of subcellular mineral and metabolite pools. Here, we describe two major radioisotope protocols used in plant biology: direct influx (DI) and compartmental analysis by tracer efflux (CATE). We focus on flux measurement of potassium (K+) as a nutrient, and ammonia/ammonium (NH3/NH4+) as a toxicant, in intact seedlings of the model species barley (Hordeum vulgare L.). These protocols can be readily adapted to other experimental systems (e.g., different species, excised plant material, and other nutrients/toxicants). Advantages and limitations of these protocols are discussed.

In planta measurement of nutrient and toxicant fluxes is essential to the study of plant nutrition and toxicity. Here, we cover radiotracer protocols for influx and efflux determination in intact plant roots, using potassium (K+) and ammonia/ammonium (NH3/NH4+) fluxes as examples. Advantages and limitations of such techniques are discussed.

Unidirectional influx and efflux of nutrients and toxicants, and their resultant net fluxes, are central to the nutrition and toxicology of plants. ...

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

Engineering

Extracting Metrics for Three-dimensional Root Systems: Volume and Surface Analysis from In-soil X-ray Computed Tomography Data

Plant roots play a critical role in plant-soil-microbe interactions that occur in the rhizosphere, as well as processes with important implications to climate change and crop management. Quantitative size information on roots in their native environment is invaluable for studying root growth and environmental processes involving plants. X-ray computed tomography (XCT) has been demonstrated to be an effective tool for in situ root scanning and analysis. We aimed to develop a costless and efficient tool that approximates the surface and volume of the root regardless of its shape from three-dimensional (3D) tomography data. The root structure of a Prairie dropseed (Sporobolus heterolepis) specimen was imaged using XCT. The root was reconstructed, and the primary root structure was extracted from the data using a combination of licensed and open-source software. An isosurface polygonal mesh was then created for ease of analysis. We have developed the standalone application imeshJ, generated in MATLAB1, to calculate root volume and surface area from the mesh. The outputs of imeshJ are surface area (in mm2) and the volume (in mm3). The process, utilizing a unique combination of tools from imaging to quantitative root analysis, is described. A combination of XCT and open-source software proved to be a powerful combination to noninvasively image plant root samples, segment root data, and extract quantitative information from the 3D data. This methodology of processing 3D data should be applicable to other material/sample systems where there is connectivity between components of similar X-ray attenuation and difficulties arise with segmentation.

A methodology for obtaining visual and quantitative root structure information from X-ray computed tomography data acquired in-soil is presented.

Plant roots play a critical role in plant-soil-microbe interactions that occur in the rhizosphere, as well as processes with important implications to ...

High-pressure, High-temperature Deformation Experiment Using the New Generation Griggs-type Apparatus

In order to address geological processes at great depths, rock deformation should ideally be tested at high pressure (&#62; 0.5 GPa) and high temperature (&#62; 300 &#176;C). However, because of the low stress resolution of current solid-pressure-medium apparatuses, high-resolution measurements are today restricted to low-pressure deformation experiments in the gas-pressure-medium apparatus. A new generation of solid-medium piston-cylinder (&#34;Griggs-type&#34;) apparatus is here described. Able to perform high-pressure deformation experiments up to 5 GPa and designed to adapt an internal load cell, such a new apparatus offers the potential to establish a technological basis for high-pressure rheology. This paper provides video-based detailed documentation of the procedure (using the &#34;conventional&#34; solid-salt assembly) to perform high-pressure, high-temperature experiments with the newly designed Griggs-type apparatus. A representative result of a Carrara marble sample deformed at 700 &#176;C, 1.5 GPa and 10-5 s-1 with the new press is also given. The related stress-time curve illustrates all steps of a Griggs-type experiment, from increasing pressure and temperature to sample quenching when deformation is stopped. Together with future developments, the critical steps and limitations of the Griggs apparatus are then discussed.

Rock deformation needs to be quantified at high pressure. A description of the procedure to perform deformation experiments in a newly designed solid-medium Griggs-type apparatus is here given. This provides technological basis for future rheological studies at pressures up to 5 GPa.

In order to address geological processes at great depths, rock deformation should ideally be tested at high pressure (&#62; 0.5 GPa) and high temperature ...

High Pressure Single Crystal Diffraction at PX^2

In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the GSECARS 13-BM-C beamline at the Advanced Photon Source. The DAC program at 13-BM-C is part of the Partnership for Extreme Xtallography (PX^2) project. BX-90 type DACs with conical-type diamond anvils and backing plates are recommended for these experiments. The sample chamber should be loaded with noble gas to maintain a hydrostatic pressure environment. The sample is aligned to the rotation center of the diffraction goniometer. The MARCCD area detector is calibrated with a powder diffraction pattern from LaB6. The sample diffraction peaks are analyzed with the ATREX software program, and are then indexed with the RSV software program. RSV is used to refine the UB matrix of the single crystal, and with this information and the peak prediction function, more diffraction peaks can be located. Representative single crystal diffraction data from an omphacite (Ca0.51Na0.48)(Mg0.44Al0.44Fe2+0.14Fe3+0.02)Si2O6 sample were collected. Analysis of the data gave a monoclinic lattice with P2/n space group at 0.35 GPa, and the lattice parameters were found to be: a = 9.496 &#177;0.006 &#197;, b = 8.761 &#177;0.004 &#197;, c = 5.248 &#177;0.001 &#197;, &#946; = 105.06 &#177;0.03&#186;, &#945; = &#947; = 90&#186;.

In this report, we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell at the GSECARS 13-BM-C beamline at the Advanced Photon Source. ATREX and RSV programs are used to analyze the data.

In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the ...

Chemistry

Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder microdiffraction two-dimensional (2D) maps at beamline 12.3.2 of the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. Measurements can be performed on any sample that is less than 10 cm x 10 cm x 5 cm, with a flat exposed surface. The experimental geometry is calibrated using standard materials (elemental standards for XRF, and crystalline samples such as Si, quartz, or Al2O3 for diffraction). Samples are aligned to the focal point of the x-ray microbeam, and raster scans are performed, where each pixel of a map corresponds to one measurement, e.g., one XRF spectrum or one diffraction pattern. The data are then processed using the in-house developed software XMAS, which outputs text files, where each row corresponds to a pixel position. Representative data from moissanite and an olive snail shell are presented to demonstrate data quality, collection, and analysis strategies.

We describe a beamline setup meant to carry out rapid two-dimensional x-ray fluorescence and x-ray microdiffraction mapping of single crystal or powder samples using either Laue (polychromatic radiation) or powder (monochromatic radiation) diffraction. The resulting maps give information about strain, orientation, phase distribution, and plastic deformation.

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder ...

Visualization of Failure and the Associated Grain-Scale Mechanical Behavior of Granular Soils under Shear using Synchrotron X-Ray Micro-Tomography

The rapid development of X-ray imaging techniques with image processing and analysis skills has enabled the acquisition of CT images of granular soils with high-spatial resolutions. Based on such CT images, grain-scale mechanical behavior such as particle kinematics (i.e., particle translations and particle rotations), strain localization and inter-particle contact evolution of granular soils can be quantitatively investigated. However, this is inaccessible using conventional experimental methods. This study demonstrates the exploration of the grain-scale mechanical behavior of a granular soil sample under triaxial compression using synchrotron X-ray micro-tomography (&#956;CT). With this method, a specially fabricated miniature loading apparatus is used to apply confining and axial stresses to the sample during the triaxial test. The apparatus is fitted into a synchrotron X-ray tomography setup so that high-spatial resolution CT images of the sample can be collected at different loading stages of the test without any disturbance to the sample. With the capability of extracting information at the macro scale (e.g., sample boundary stresses and strains from the triaxial apparatus setup) and the grain scale (e.g., grain movements and contact interactions from the CT images), this procedure provides an effective methodology to investigate the multi-scale mechanics of granular soils.

The protocol describes procedures to acquire high-spatial resolution computed tomography (CT) images of a granular soil during triaxial compression, and to apply image processing techniques to these CT images to explore the grain-scale mechanical behavior of the soil under loading.

The rapid development of X-ray imaging techniques with image processing and analysis skills has enabled the acquisition of CT images of granular soils ...

An Externally-Heated Diamond Anvil Cell for Synthesis and Single-Crystal Elasticity Determination of Ice-VII at High Pressure-Temperature Conditions

The externally-heated diamond anvil cell (EHDAC) can be used to generate simultaneously high-pressure and high-temperature conditions found in Earth&#8217;s and planetary interiors. Here we describe the design and fabrication of the EHDAC assemblies and accessories, including ring resistive heaters, thermal and electrical insulating layers, thermocouple placement, as well as the experimental protocol for preparing the EHDAC using these parts. The EHDAC can be routinely used to generate megabar pressures and up to 900 K temperatures in open air, and potentially higher temperatures up to ~1200 K with a protective atmosphere (i.e., Ar mixed with 1% H2). Compared with a laser-heating method for reaching temperatures typically &#62;1100 K, external heating can be easily implemented and provide a more stable temperature at &#8804;900 K and less temperature gradients to the sample. We showcased the application of the EHDAC for synthesis of single crystal ice-VII and studied its single-crystal elastic properties using synchrotron-based X-ray diffraction and Brillouin scattering at simultaneously high-pressure high-temperature conditions.

This work focuses on the standard protocol for preparing the externally-heated diamond anvil cell (EHDAC) for generating high-pressure and high-temperature (HPHT) conditions. The EHDAC is employed to investigate materials in Earth and planetary interiors under extreme conditions, which can be also used in solid state physics and chemistry studies.

The externally-heated diamond anvil cell (EHDAC) can be used to generate simultaneously high-pressure and high-temperature conditions found in ...

Determining the Mechanical Strength of Ultra-Fine-Grained Metals

The mechanical strengthening of metals is the long-standing challenge and popular topic of materials science in industries and academia. The size dependence of the strength of the nanometals has been attracting a lot of interest. However, characterizing the strength of materials at the lower nanometer scale has been a big challenge because the traditional techniques become no longer effective and reliable, such as nano-indentation, micropillar compression, tensile, etc. The current protocol employs radial diamond-anvil cell (rDAC) X-ray diffraction (XRD) techniques to track differential stress changes and determine the strength of ultrafine metals. It is found that ultrafine nickel particles have more significant yield strength than coarser particles, and the size strengthening of nickel continues down to 3 nm. This vital finding immensely depends on effective and reliable characterizing techniques. The rDAC XRD method is expected to play a significant role in studying and exploring nanomaterial mechanics.

The protocol presented here describes the high-pressure radial diamond-anvil-cell experiments and analyzing the related data, which are essential for obtaining the mechanical strength of the nanomaterials with a significant breakthrough to the traditional approach.

The mechanical strengthening of metals is the long-standing challenge and popular topic of materials science in industries and academia. The size ...

Single Crystal and Powder X-ray Diffraction

Source: Tamara M. Powers, Department of Chemistry, Texas A&#38;M University&#160;
X-ray crystallography is a technique that uses X-rays to study the structure of molecules. X-ray diffraction (XRD) experiments are routinely carried out with either single-crystal or powdered samples.
Single-crystal XRD:
Single-crystal XRD allows for absolute structure determination. With single-crystal XRD data, the exact atomic positions can be observed, and thus bond lengths and angles can be determined. This technique provides the structure within a single crystal, which does not necessarily represent the bulk of the material. Therefore, additional bulk characterization methods must be utilized to prove the identity and purity of a compound.
Powder XRD:
Unlike single-crystal XRD, powder XRD looks at a large sample of polycrystalline material and therefore is considered a bulk characterization technique. The powder pattern is considered a &#34;fingerprint&#34; for a given material; it provides information about the phase (polymorph) and crystallinity of the material. Typically, powder XRD is used to study minerals, zeolites, metal-organic frameworks (MOFs), and other extended solids. Powder XRD can also be used to establish bulk purity of molecular species.
Previously, we have seen how to grow X-ray quality crystals (see video in Essentials of Organic Chemistry series). Here we will learn the principles behind XRD. We will then collect both single-crystal and powder data on Mo2(ArNC(H)NAr)4, where Ar = p-MeOC6H5.

Source: Tamara M. Powers, Department of Chemistry, Texas A&#38;M University&#160;
X-ray crystallography is a technique that uses X-rays to study the ...

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