Design InnovationDESIGN INNOVATION PAPERS Design of a Magnetic Resonance Imaging Compatible Metallic Pressure Vessel Matthew Ouellette, Hui

Han, Bryce MacMillan, Frederic Goora, Rodney MacGregor, Marwan Hassan and Bruce J. Balcom [+-] Author Affiliations Matthew Ouellette MRI Research Centre, Department of Physics, Mechanical Engineering Department, University of New Brunswick, Fredericton, New Brunswick, E3B 5A3, Canada Rodney MacGregor MRI Research Centre, Department of Physics, University of New Brunswick, Fredericton, New Brunswick, E3B 5A3, Canada Marwan Hassan Mechanical Engineering Department, University of New Brunswick, Fredericton, New Brunswick, E3B 5A3, Canada Bruce J. Balcom MRI Research Centre, Department of Physics, University of New Brunswick, Fredericton, New Brunswick, E3B 5A3, Canada e-mail: bjb@unb.ca Corresponding author. Contributed by the Pressure Vessel and Piping Division of ASME for publication in the Journal of Pressure Vessel Technology. Manuscript received March 27, 2012; final manuscript received February 4, 2013; published online June 11, 2013. Assoc. Editor: Allen C. Smith. J. Pressure Vessel Technol. 135(4), 045001 (Jun 11, 2013) (7 pages)doi:10.1115/1.4023728History: Received March 27, 2012; Revised February 04, 2013

Article References Figures Tables Abstract Abstract | Introduction | MRI Background | MRI-Compatible Metallic Pressure Vessel Design | Design and Constraints | Imaging Results | Conclusion | Acknowledgements | References High-pressure measurements in most scientific fields rely on metal vessels, a consequence of the superior tensile strength of metals. Magnetic resonance imaging in conjunction with metallic pressure vessels has recently been introduced. Magnetic resonance imaging with compatible metallic pressure vessels is a very general concept. This paper outlines the specifics of the development and design of these vessels. Metallic pressure vessels not only provide inherently high tensile strengths and efficient temperature control, they also permit optimization of the radio-frequency probe sensitivity. The design and application of magnetic resonance imaging compatible pressure vessels is illustrated through a rock core holder fabricated using nonmagnetic stainless steel. Water flooding through a porous rock at elevated pressure and temperature is shown as an example of its applications. High-pressure magnetic resonance plays an indispensable role in several scientific fields; this work will open new avenues of investigation for high-pressure material science magnetic resonance imaging. FIGURES IN THIS ARTICLE <>

Introduction Abstract | Introduction | MRI Background | MRI-Compatible Metallic Pressure Vessel Design | Design and Constraints | Imaging Results | Conclusion | Acknowledgements | References Over the past half century high-pressure magnetic resonance (MR) has played an important role in many areas of physics and chemistry [1-6]. Specifically MR measurements at high pressure and variable temperature provide unique information about the microscopic behavior of liquids [2,3]. Magnetic resonance imaging (MRI) has revolutionized clinical diagnostic imaging and its use exploring and understanding other natural science systems is expanding. There is clear merit in combining MRI with high pressure and temperature control for materials investigation. We have previously introduced high-pressure magnetic resonance imaging using metallic vessels from a magnetic resonance point of view [7,8]. This article describes the process of designing these vessels, the ultimate design goals, and their effects on the design and fabrication. The material selections, sizing (diameter, wall thickness, length), sealing mechanisms, and radio-frequency (RF) probe design are all governed by the design goals and unique limitations imposed by MRI. For a pressure vessel the most notable design goals are the design pressure and temperature range. The metal vessel encloses a pressurized RF probe with the metal enclosure functioning as an RF shield. The naturally high thermal conductivity of metals allows the sample space temperature to be monitored and controlled by regulating the outside temperature of the vessel. The metallic pressure vessels imagined are very general in concept; they may be closed vessels of various designs including chemical reaction vessels, high-pressure pipes, or rock core holders with radial pressure application. In this article a rock core holder is used as a specific example of a metallic pressure vessel. A core holder is employed to maintain a cylindrical rock sample at high pressure and specified temperature in order to recreate petroleum reservoir conditions. The design pressure and temperature for this core holder were chosen to be common, but not extreme, conditions of 6.9MPa (1000psi) and 50C. Once a rock core sample is at reservoir conditions, MRI can be employed to analyze the fluid behavior to obtain information about the nature of the reservoir. As an illustration of this utility, water flooding a porous rock under pressure and temperature control is monitored by MRI.

A limited number of high-pressure MRI studies have previously been reported [9-12]. These studies almost universally employ nonmetallic polymer composite cells that fit into an existing MRI RF probe. These measurements are hindered by low sensitivity of the RF probe due to the distance between the probe and sample under investigation [9-11] as well as inefficient temperature control due to low thermal conductivity of the polymer [9-11]. MRI Background Abstract | Introduction | MRI Background | MRI-Compatible Metallic Pressure Vessel Design | Design and Constraints | Imaging Results | Conclusion | Acknowledgements | References Magnetic resonance occurs for atomic nuclei having odd numbers of protons or neutrons, and thus possessing a net magnetic moment. Hydrogen is the most commonly examined nuclei; MRI is most sensitive to hydrogen, and most desirably H2O and hydrocarbons can be investigated. In the presence of a static magnetic field (B0), the magnetic moments are polarized resulting in a net magnetization vector (M0) in the B0 direction. The nuclear spins can be excited with a radio-frequency (RF) field (B1) applied perpendicular to B0 at the Larmor frequency given by [13]: (1)f 0 =B 0 Where is the gyromagnetic ratio and B0 is the magnetic field strength. The gyromagnetic ratio is a constant and depends on the nuclei being examined, in the case of 1H it is 42.58MHz/T. RF excitation causes M0 to depart from equilibrium and precess about the static field. Precessing magnetization induces an electrical potential difference in the RF coil when switched to reception mode. The system will return to equilibrium with characteristic MRI signal relaxation times T1, T2, and T2*. In the case of a centric scan SPRITE MRI method, commonly employed for quantitative studies of fluids in porous media [14], the local image intensity is given by (2)S=M 0 exp(t p T 2 )sin Where tp is the phase encoding time, and is the RF rotation angle. The net magnetization vector M0 is proportional to quantity of nuclei; therefore the induced voltage in the RF probe will be directly proportional to local fluid quantity 0. (3)S 0 exp(t p T 2 )sin Switched magnetic field gradients are employed to spatially resolve the signal in one, two, or three dimensions [15,16]. The signal intensity at each pixel or voxel will be governed by Eq. (3); fluid quantity and relaxation time information is measured and spatially resolved. MRI-Compatible Metallic Pressure Vessel Design Abstract | Introduction | MRI Background | MRI-Compatible Metallic Pressure Vessel Design | Design and Constraints | Imaging Results | Conclusion | Acknowledgements | References

Figure 1(a) shows a schematic of a general MRI compatible metallic pressure vessel. The metallic vessel encloses a pressurized MRI RF probe with the metal enclosure functioning as an RF shield. The metallic pressure vessel, surrounded by a temperature control coil, fits inside a standard gradient bore on an MRI spectrometer. Figure 1(b) shows a conventional nonmetallic vessel. The RF coil is placed outside of the vessel. Pressure Vessel Stresses. Conventional (non-MRI) laboratory studies at high pressure rely on metal vessels given their superior tensile strength. The high tensile strength of metals permits larger macroscopic volumes to be studied by MRI. As the size of a pressure cell increases, the required yield strength of the cell must increase proportionally to maintain the same maximum internal pressure. For a thick-walled cylindrical pressure vessel the radial stress r and circumferential stress vary as a function of radius r as *17+ (4) r =P(r 2 i r 2 o r 2 i )(r 2 i r 2 +1) (5) =P(r 2 i r 2 o r 2 i )(r 2 i r 2 +1) where P is the pressure difference from ambient pressure, ri is the inner radius of the cylinder, and ro is the outside radius. Longitudinal stress z in the cylinder is constant and described as (6) z =P(r 2 i r 2 o r 2 i ) The maximum allowable stress in the cylinder will be a yield criterion stress divided by a safety factor SF. For this design a conservative safety factor of three was assumed. The most common yield criterion for ductile materials is the Von Mises stress VM. The Von Mises stress assumes that failure occurs when the energy of distortion reaches the same energy for yield/failure in uniaxial tension. Mathematically this is expressed as (7) VM =1 2 *( r z ) 2 +( r ) 2 +( z ) 2 + The maximum Von Mises stress will occur on the inside wall of the cyldinder where r=ri. The high yield strength of stainless steel makes it a near universal choice for conventional pressure vessels. A variety of metals may be employed for fabricating the cylindrical vessel including aluminum, nonmagnetic stainless steel alloys, brass, and titanium. The physical properties relevant to MRI compatible pressure vessels are shown in Table 1 [18,19]. Stainless steel has a very high tensile strength, 400MPa *18+, twice that of aluminum. For a nonmetallic MRI-compatible pressure vessel thicker walls are required because of the inherently lower tensile strength of the materials. For a constant inside radius (sample space) and design pressure, the wall thickness required (rori) will change, depending on the strength of material used. The wall thickness required for an aluminum vessel is roughly twice as large as that of a vessel made of stainless

steel, and vessel made of polyether ether ketone (PEEK) is nearly four times the thickness of a stainless steel vessel. Temperature Control. Operation at variable pressure and temperature are critical requirements for pressure vessels. Temperature control is consistently problematic in MRI since MR observable fluids (notably water) cannot be readily employed. The water will superimpose as signal over the sample being measured, where a metal vessel will shield this signal. Commercially available solutions, such as those available from Temco [11,12] involve circulating fluid under high pressure through the pressure vessel. The confining fluid must be temperature controlled, pressurized, and circulated. This is a complicated and expensive solution because of the specialized pumps and equipment required. One may however readily exploit the high thermal conductivity of metals, forming the wall of a metallic pressure vessel, for a much simpler and more passive method of temperature control. The high thermal conductivity of metals as outlined in Table 1, allow the sample temperature inside the vessel to be manipulated by controlling the outside temperature of the vessel and letting the system reach equilibrium. The metallic vessel can be modeled as a hollow cylinder, with the instantaneous rate of heat transfer per unit length into the cylinder Q (W/m) a function of inside and outside radius ri and ro, inside and outside temperatures Ti and To, and thermal conductivity k as follows [20]: (8)Q=2k(T i T o ) ln(r o /r i ) If the outside temperature To is held constant, heat will be deposited into the sample space temperature Ti, at rate Q. The rate of heat transfer will decay in proportion to the temperature gradient shrinking as inside temperature approaches the outside. At steady state the heat equation for a hollow cylinder is given as (9)d dr (rdT dr )=0 Assuming a constant outside temperature, the general solution for temperature as a function of radius at steady state is (10)T(r)=Qr i k ln(r o r )+T o Substituting Eqs. (8) into (10) shows that at steady state (after a long enough time period in this case), the outside temperature will be equal to the inside. The high thermal conductivity of metals allows for a high rate of heat transfer; therefore the sample approaches steady state relatively quickly. This method is not possible with conventional MRI-compatible pressure vessels made of polymers with low thermal conductivities. The temperature control setup for the metallic core holder is much simpler compared to commercial solutions. Applying nitrogen gas from a gas cylinder pressurizes the sample space. The regulation of the outside temperature is achieved by pumping temperature-regulated water through thermally conductive tubing in contact with the exterior of the vessel. Water is a natural choice given the high

thermal capacity of water and ease of handling water flow. Unlike nonmetallic pressure vessels, one need not be concerned about MRI detection of the external water by the RF probe since the metallic vessel acts as an RF shield. This temperature control strategy is simple, robust and advantageous because it separates temperature control from pressure regulation. The Nitronic 60 nonmagnetic stainless steel core holder was tested for temperature control. The temperature was monitored with a thermocouple attached inside the sample space. As expected, temperature changed exponentially with time. To reach a sample space temperature of 50C from room temperature required an hour. Probe Sensitivity. MRI is based on the manipulation and detection of nuclear magnetism, and nuclear magnetism is a relatively weak physical effect. This leads to MRI being a relatively insensitive measurement technique, but the metallic vessel design offers two unique benefits that help greatly increase the sensitivity of the MRI experiment. Placement of the RF coil in close proximity to the sample space maximizes the probe sensitivity, and the metallic vessel acts as an electromagnetic interference (EMI) shield for the RF probe reducing background interference and noise. In previous work the background noise level was measured for the probe without any RF shielding, the probe enclosed within the steel core holder, and the probe enclosed in a typical copper shield. The background noise for the metallic vessel was found to be an order of magnitude less than the unshielded case [7]. The background noise for the conventional copper shield was roughly twice the metallic vessel [7]. The principle of reciprocity suggests that maximizing the RF coil sensitivity requires maximizing the RF magnetic field B1 per unit current in the sample space [21]. The B1 field (at the center of the coil) per unit current is inversely proportional to the characteristic size of the probe coil [22]. For example the magnetic field B at the center of a current loop for a circular coil with diameter D is where 0 denotes the vacuum magnetic permeability and I is the total current in the loop. The ultimate sensitivity S of an MRI experiment at sample temperature Ts and RF probe temperature TRF is described as [22] (12)SB 1 I 1 T s T RF From Eq. (11), the ratio of B1/I is inversely proportional to the characteristic size of the RF coil, which when combined with Eq. (12) gives the relationship (13)S1 D 1 T s T RF The value of 1/D is at least two times larger for a metallic vessel than for nonmetallic vessel and more likely a factor of 4 because the probe is inside the vessel, not outside.

One must consider that the RF probe in a metallic vessel will be maintained at the sample temperature Ts instead of the magnet bore temperature Tmag and as a consequence will have increased thermal noise as the sample temperature is increased as suggested by Eq. (13). This is fundamental to the design and a potential drawback compared to the conventional approach. Calculating the sensitivity to compare the effects in the metallic vessel (favorable 1/D, less favorable TRF=Ts) to those in the nonmetallic one (less favorable 1/D, favorable TRF=Tmag) show the metallic vessel to be highly favorable. Decreasing the sample temperature below ambient lab temperature improves the situation where TRF=Ts. The thermal noise does not balance the effects of the increased sensitivity of the RF probe until the sample temperature reaches 3600C. At the design temperature of 50C, the ultimate sensitivity is 3.8 times greater for the metallic vessel versus the nonmetallic case. Both of these results prove the RF probe for a metallic vessel to be very sensitive and therefore very effective. Eddy Current Effects. Switched magnetic field gradients are essential to spatial encoding and motion sensitization in modern MRI. As the magnetic field gradient switches, eddy currents will circulate in metals and may distort the desired magnetic field in the sample space. We have previously examined the eddy current problem associated with MR imaging inside conductive metallic structures [8], and how it may be solved by magnetic field gradient measurement and data correction. Eddy currents induced in a cylindrical metal vessel decay exponentially, with a time constant dominated by the following term [8,23]: (14)=K where and are the electrical conductivity and magnetic permeability of the material, K is a constant, and represents a geometric factor. Illustrated in Table 1, a stainless steel vessel compared to aluminum reduces electrical conductivity and therefore eddy current time constants by a factor of almost 30 [18,19]. Gradient waveforms were simulated for both Nitronic 60 stainless steel and aluminum cells using CST EM Studio [24]. Appropriate geometries were selected for comparison with magnetic field gradient waveform measurements [25]. The simulations showed aluminum had a severe eddy current problem while the Nitronic 60 stainless steel did not. In the case of Nitronic 60 the eddy current effect decayed within 0.85ms, while for aluminum it lasted 32ms. Simulation and experiments agreed very well; the difference between gradient rise times measured experimentally and determined through simulation was less than 5%. Design and Constraints Abstract | Introduction | MRI Background | MRI-Compatible Metallic Pressure Vessel Design | Design and Constraints | Imaging Results | Conclusion | Acknowledgements | References A core holder was chosen as an application of the MRI compatible metallic pressure vessel concept. A core holder is employed to maintain a cylindrical rock core sample at high pressure and specified temperature in order to recreate petroleum reservoir conditions. A core holder applies a static radial

pressure and variable axial pressure to force a flow in the longitudinal direction for measurements. In this case a design pressure and temperature of 6.9MPa (1000psi) and 50C was chosen, with a safety factor of three chosen for the design. Figure 2(a) depicts a core holder embodying the principles outlined in Fig. 1(a). The metallic vessel wall encloses an RF probe that in turn contains a sample. Access through the end plugs is provided through threaded holes for fluid inflow/outflow and electrical connection to the RF probe. The type of RF probe employed will vary depending on the style of magnet employed. In the case of superconducting magnets, a birdcage or saddle coil is used [22]. Figure 2(b) shows the construction of the probe. The RF probe is constructed of two concentric hollow cylinders with the RF coil embedded in the diametrical clearance between them. The RF probe assembly is sealed with a high strength epoxy impermeable to water. A conventional RF shield is not required since the vessel wall performs this function. Figure 2(c) shows a photo of the MRI-compatible core holder fabricated from Nitronic 60 stainless steel. The core plug sample is held by heat shrink tubing and an Aflas polymer sleeve to make a connection to the inlet and outlet fluid distribution plugs. The encapsulated sample is positioned inside the RF probe. The entire assembly goes into the metal vessel. The vessel is sealed at the ends by o-rings on the plugs. Radial pressure is exerted on the sample through the containment sleeve by pressurizing the internal space. The Aflas sleeve and heat shrink isolate the sample from the pressurizing fluid. The internal space is pressurized by introducing a fluid nonobservable to MR (e.g., fluorinated oil or gas) through external connection by means of a hydraulic pump or gas cylinder; in this work nitrogen gas was chosen to pressurize the core holder. Axial flow through the sample is provided by fluid pumped through fluid distribution plugs at each end of the sample. Material Choices. As discussed earlier, an optimal material for construction of the body of the vessel will offer exceptional tensile strength, low electrical conductivity, and relatively high thermal conductivity. The material with the best balance of these characteristics was chosen to be an alloy of stainless steel, Nitronic 60 stainless steel (McMaster Carr, OH). It is an austenitic steel making it nonmagnetic, while still offering the benefits of high tensile strength (400MPa), low electrical conductivity (1.39106S/m) and relatively high thermal conductivity (16W/mK), compared to other possible materials shown in Table 1 [18,19]. For construction of the RF probe and body inside the pressure vessel, materials are chosen to minimize hydrogen background signal. Early designs of the core holder showed issues with background signal from the materials used, specifically the epoxy and material used for construction of the RF probe as shown in Fig. 2(b). For the first version, the epoxy employed was a marine epoxy (West Systems, MI) and the RF probe body was made of G-10 fiberglass (McMaster Carr, OH) [7]. Figure 3(a) shows a 1D profile of the longitudinal (Z) axis of the first version core holder with a rock core plug present. It is a core flooding experiment where water floods the rock from the left to right in the image. It can be seen that the background signal is of the same order of magnitude as the sample. The

background signal originates with the marine epoxy and other polymers in the RF probe. The strength of the background signal will be very temperature sensitive; the signal lifetime of polymers are generally longer at elevated temperatures [26]. It is possible to record and average the background and then subtract it from the experimental profiles. This methodology is relatively easy but not desirable; zero or mean zero background signals would be ideal. To further investigate the background signal a 2D image of the transverse plane (XY) of a water saturated Berea rock plug was recorded and shown in Fig. 3(b). Note the bright spot at the center of the rock core image. This is from water in the inlet/outlet tubing as seen in the side view image Fig. 2(a). At the circular edge of the rock core, image signal is slightly enhanced due to background signal from the Aflas sleeve housing the rock. There is also signal from epoxy in proximity to the eight rungs of the birdcage RF probe, where the RF B1 field is strong [22]. For the next version of the core holder, modifications were made to minimize background signal. Glassfilled PTFE (McMaster Carr, OH) instead of fiberglass G-10 was used for construction of the RF probe. As part of this research we investigated a large number of potential epoxies to determine the most suitable for construction of the RF probe. The MRI signal behavior of the epoxies was investigated to determine the epoxy with the best combination of low signal magnitude and quickly decaying signal. The optimal choice was found to be epoxy M31CL (McMaster Carr, OH). Figure 3(c) displays the results of these efforts, showing the same transverse image of a saturated rock sample in the newer version of the probe with reduced background signal. The ratio of signal from a water saturated rock sample to background signal was measured for both versions of the core holder and increased from a ratio of approximately 1:1 to 35:1 in the old versus new version. This shows how critical material selection is to the process of designing and fabricating a MRI-compatible pressure vessel; especially in the RF probe. Other Design Considerations. The design of the core holder had many constraints on physical size. The outside diameter of the core holder has a maximum limit which is the diameter of the gradient bore. The outside diameter had a minimum limit as per the required thickness for a design pressure and sample size. The inside diameter is limited by the size of the sample and the RF coil. The most common core holder sample sizes are 1.5 or 1 in. in diameter; 1 in. was chosen for this design. The RF probe requires a certain diametrical clearance between the sample and vessel wall. For the core holder shown, the probe assembly was roughly 1/2 in. thick. The length is constrained by the rock sample sizes as well as the fluid distribution plugs. Core plugs are typically several inches in length, accommodation from 0 to 3 in. lengths were considered in this design. Different designs were considered and used for the sealing of the core holder on each end. Each end has several longitudinal connections with lines/wires attached so the sealing mechanism cannot be one that rotates or else the lines and connections will become tangled. Many commercial pressure vessels use a sealing mechanism as outlined in Fig. 4(a). The size limitations of fitting inside the magnet bore prevents the utilization of a large diameter bolt circle with a face-sealing o-ring, as it is not space efficient. The sealing mechanism chosen for the core holder was an o-ring sealing similar to a piston, as shown in Fig.

4(b). This design proved to be most effective, having the benefits of no rotation of the end caps required, as well as being more space efficient relative to conventional face-sealing pressure vessels. As mentioned earlier, eddy currents and their induced magnetic fields were simulated for various metallic pressure vessels. Simulation permits rapid survey of vessel parameters such as metal selection and geometry, which would not be easily accomplished experimentally due to the associated material and machining costs. Design of the vessel involved iteration between the simulations and geometry; vessel geometry would be simulated and then modified according to the simulation results [7]. Imaging Results Abstract | Introduction | MRI Background | MRI-Compatible Metallic Pressure Vessel Design | Design and Constraints | Imaging Results | Conclusion | Acknowledgements | References As a simple example of the nonmagnetic Nitronic 60 stainless steel core holder, water flooding in a sandstone rock core was monitored with MRI. The two-dimensional centric scan Spiral SPRITE [14] was employed for test imaging. As shown in Fig. 5(a), water was driven through a dry Berea sandstone from right to left. The confining pressure and the temperature were set to 2.1MPa (300psi) and 50C, respectively. A flow rate of 0.3ml/min of water was used to flood the sample. During the flooding experiment, 2D images were acquired at intervals of 43s; the acquisition time per 2D image was 43s with four signal averages. After 40min of imbibition the rock was fully saturated. Figure 5(b) shows 1D profiles extracted from the centerline of the 2D image at intervals of 3.6min. Conclusion Abstract | Introduction | MRI Background | MRI-Compatible Metallic Pressure Vessel Design | Design and Constraints | Imaging Results | Conclusion | Acknowledgements | References This paper discusses the development of high-pressure MRI-compatible metallic vessels. Compared to conventional MRI core holders and pressure vessels, the proposed metallic pressure vessels permit much more efficient temperature control, optimized sensitivity, and act as an EMI shield. Nitronic 60 stainless steel was found to be the most effective material for the vessel with a combination of high tensile strength, relatively high thermal conductivity, and low electrical conductivity. Eddy currents are dramatically reduced using stainless steel because of its relatively low electrical conductivity compared to other metals. The sensitivity is greatly improved compared to conventional MRI compatible pressure vessels, due to the probe being inside as opposed to outside the vessel. Background signal from polymer materials inside the metal vessel are an issue, being on the same order of magnitude as sample signal in earlier versions of the vessel. Simple averaging of the background signal and subtraction was demonstrated as a short-term solution, but different material choices to minimize background signal is a better strategy. Quantitative imaging of water flooding a rock core plug in a stainless steel core holder under moderate pressure and temperature shows the potential of this methodology. MRI compatible metallic pressure vessels enable macroscopic systems at high pressure and variable temperature to be monitored by MRI.

Acknowledgements Abstract | Introduction | MRI Background | MRI-Compatible Metallic Pressure Vessel Design | Design and Constraints | Imaging Results | Conclusion | Acknowledgements | References B.J.B. thanks the Canada Chairs program for a Research Chair in MRI of Materials (20092016), NSERC of Canada for a Discovery grant, and ConocoPhillips. We thank many for their assistance and suggestions: Dr. I. Mastikhin and Dr. B. Newling, as well as M. Olive and B. Titus. We thank Adam Melanson for his investigation of water impermeable epoxies. References Abstract | Introduction | MRI Background | MRI-Compatible Metallic Pressure Vessel Design | Design and Constraints | Imaging Results | Conclusion | Acknowledgements | References 1 Benedek, B., and Purcell, M. J., 1954, Nuclear Magnetic Resonance in Liquids Under High Pressure, J. Chem. Phys., 22, pp. 20032012. [CrossRef] 2 Jonas, J., 1982, Nuclear Magnetic Resonance at High Pressure, Science, 216, pp. 11791184. [CrossRef] [PubMed] 3 Grunwaldt, J. D., Wandeler, R., and Baiker, A., 2003, Supercritical Fluids in Catalysis: Opportunities of In Situ Spectroscopic Studies and Monitoring Phase Behavior, Catal. Rev., 45, pp. 196. [CrossRef] 4 Angel, R. J., Ross, N. L., Seifert, F., and Fliervoet, T. F., 1996, Structural Characterization of Penta Coordinate Silicon in a Calcium Silicate, Nature, 384, pp. 441444. [CrossRef] 5 Horvath, I. T., and Miuar, J. M., 1991, NMR Under High Gas Pressure, Chem. Rev., 91, pp. 13391351. [CrossRef] 6 Lee, S. K., Mibe, K., Fei, Y. W., Cody, G. D., and Mysen, B. O., 2005, Structure of B2O3 Glass at High Pressure: A 11B Solid-State NMR Study, Phys. Rev. Lett., 94, 165507-1, 4. [CrossRef] 7

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