Patent Grant
11714079
Water injection is a common technique used in oil production to increase the yield of hydrocarbons from a reservoir. The interactions between the various phases in the reservoir (e.g., oil, water, brines, calcite rock, and gas) can greatly affect yield of the recovered hydrocarbons. For example, by controlling the salinity and the ionic strength of the injected solution, the wettability of rock formations in the reservoir can be changed to improve recovery. To further improve the yield of hydrocarbons, various spectroscopic techniques such as SFG spectroscopy have been used to understand the nature of the interactions between the phases in the reservoir and characterize the chemical and molecular structure and interfaces of the phases.
In one aspect, one or more embodiments disclosed herein relate to a pressure cell for SFG spectroscopy. The pressure cell includes a metal pressure chamber that includes a liquid sample holder that retains a liquid sample, a removable lid that seals against a base to enclose the liquid sample holder in an interior of the metal pressure chamber, a window in the removable lid that allows the liquid sample to be optically accessed from an exterior of the metal pressure chamber, a sample inlet that flows the liquid sample from the exterior of the metal pressure chamber to the liquid sample holder in the interior of the metal pressure chamber at a predetermined flow rate, and a sample outlet that flows the liquid sample from the liquid sample holder to the exterior of the metal pressure chamber. The pressure cell further includes: a heating stage, disposed in the interior of the metal pressure chamber, that heats the liquid sample; an ultrasonic stage, disposed in the interior of the metal pressure chamber, that emulsifies the liquid sample; a chamber pump, connected to the interior of the metal pressure chamber, that pressurizes the interior of the metal pressure chamber; and a controller that controls the chamber pump, the ultrasonic stage, and the heating stage to control a pressure of the interior of the metal pressure chamber, an emulsification of the liquid sample, and a temperature of the liquid sample, respectively.
In another aspect, one or more embodiments disclosed herein relate to a system for performing SFG spectroscopy. The system includes: a pressure cell and a sum frequency generation microscope. The pressure cell includes a metal pressure chamber that includes a liquid sample holder that retains a liquid sample, a removable lid that seals against a base to enclose the liquid sample holder in an interior of the metal pressure chamber, a window in the removable lid that allows the liquid sample to be optically accessed from an exterior of the metal pressure chamber, a sample inlet that flows the liquid sample from the exterior of the metal pressure chamber to the liquid sample holder in the interior of the metal pressure chamber at a predetermined flow rate, and a sample outlet that flows the liquid sample from the liquid sample holder to the exterior of the metal pressure chamber. The pressure cell further includes: a heating stage, disposed in the interior of the metal pressure chamber, that heats the liquid sample; an ultrasonic stage, disposed in the interior of the metal pressure chamber, that emulsifies the liquid sample; a chamber pump, connected to the interior of the metal pressure chamber, that pressurizes the interior of the metal pressure chamber; and a controller that controls the chamber pump, the ultrasonic stage, and the heating stage to control a pressure of the interior of the metal pressure chamber, an emulsification of the liquid sample, and a temperature of the liquid sample, respectively. The sum frequency generation microscope includes: a first light source that generates light of a first variable frequency; a second light source that generates light of a second frequency; and a detector that detects light.
In another aspect, one or more embodiments disclosed herein relate to a method of performing SFG spectroscopy. The method includes: sealing a liquid sample holder in an interior of a metal pressure chamber that includes a base and a removable lid; flowing a liquid sample from an exterior of the metal pressure chamber, thorough a sample inlet, to the liquid sample holder in the interior of the metal pressure chamber at a predetermined flow rate; emulsifying the liquid sample with an ultrasonic stage; heating the liquid sample with a heating stage; pressurizing the interior of the metal pressure chamber with a chamber pump that is connected to the interior of the metal pressure chamber; illuminating a surface of the liquid sample with light of a first variable frequency and light of a second frequency through a window of the metal pressure chamber; collecting, through the window, light of a third frequency that is the sum of the first variable frequency and the second frequency from the surface of the liquid sample; and flowing the liquid sample from the liquid sample holder, through a sample outlet, to the exterior of the metal pressure chamber.
Other aspects and advantages will be apparent from the following description and the appended claims.
Specific embodiments of the present disclosure will now be described in detail with reference to the accompanying figures. Like elements in the various figures are denoted by like reference numerals for consistency.
Numerous specific details are set forth in the following detailed description in order to provide a more thorough understanding of embodiments of the present disclosure. However, it will be apparent to one of ordinary skill in the art that the present disclosure may be practiced without these specific details. In other instances, well-known features have not been described in detail to avoid unnecessarily complicating the description.
Throughout the application, ordinal numbers (e.g., first, second, third, etc.) may be used as an adjective for an element (i.e., any noun in the application). The use of ordinal numbers is not to imply or create a particular ordering of the elements nor to limit any element to being only a single element unless expressly disclosed, such as by the use of the terms “before,” “after,” “single,” and other such terminology. Rather the use of ordinal numbers is to distinguish between the elements. By way of an example, a first element is distinct from a second element, and the first element may encompass more than one element and succeed (or precede) the second element in an ordering of elements.
In general, embodiments disclosed herein provide an apparatus, a system, and a method for performing sum frequency generation (SFG) spectroscopy under simulated reservoir and dynamic conditions to characterize the molecular and chemical structures and interfaces of an oil/brine sample. For example, as shown in
To improve the effectiveness of the injection recovery technique, the microscopic characteristics of, and interactions between, the hydrocarbons 108, the injection solution, and the rock formations of the reservoir 102 may be studied. Examples of such interactions may include surface charge interaction, ionic exchange, and rock dissolution. SFG spectroscopy may be used to probe the fluid/fluid or fluid/rock interactions and to characterize the chemical and molecular structures and interfaces of a liquid sample, discussed in further detail below. Accordingly, one or more embodiments disclosed herein relate to an apparatus, a system, and a method of studying a liquid sample with SFG spectroscopy in a simulated high temperature and high pressure reservoir environment. Alternatively, other optical techniques (e.g., difference frequency generation (DFG) spectroscopy, Raman spectroscopy) may be used in conjunction with embodiments disclosed herein.
In one or more embodiments, a liquid sample may be extracted from a subsurface facility (e.g., the reservoir 102). For example, a live oil sample may be obtained from the oil well 106. Furthermore, to more closely recreate the actual fluids found downhole in the well (e.g., compositions previously determined using a modular formation dynamic tester (MDT) technique), gases such as gaseous hydrocarbons, hydrogen sulfide, and the like may be remixed into the live oil sample. Alternatively, or in addition, aqueous solutions may be remixed into the live oil sample to recreate the actual fluids found downhole in the well, as described below.
In one or more embodiments, liquid samples collected from the reservoir may be separated into two phases: an organic phase (i.e., primarily hydrocarbons 108 of the live oil sample) and the second component includes an aqueous phase (i.e., primarily water). Then, the two phases may be remixed with a predetermined ratio and/or predetermine level of emulsification. Thus, the liquid sample to be studied may be a synthetic brine (i.e., prepared in a laboratory) comprising the remixed hydrocarbons 108 and an aqueous solution.
The term “brine” is defined as a mixture comprising two or more immiscible liquids. A first component of the brine is dispersed in a second component of the brine. In one or more embodiments, the dispersed first component includes an organic phase (i.e., primarily hydrocarbons) and the second component includes an aqueous phase (i.e., primarily water). Alternatively, the phases of the first and second components may be reversed. In one or more embodiments, the liquid sample may be a brine comprising gaseous hydrocarbons, liquid hydrocarbons, solid hydrocarbons, salts, metals, impurities, water, an aqueous solution, and any combination thereof.
The first light beam is centered at a first variable frequency f1 that may correspond with an energy level of a molecular vibrational mode that occurs in the sample (e.g., corresponds to an infrared wavelength of light). The first variable frequency f1 may be continuously or discretely changed (e.g., with a tunable light source, a filtered light source, a spectrometer, or the like) to probe different energy levels of different molecular vibrational modes in the sample. The first light beam may be incident at an angle of 60° with respect to the normal vector of the sample surface.
The second light beam is centered at a second frequency f2 that is different from the first variable frequency f1 and may correspond to a virtual energy state (e.g., corresponds to a visible wavelength of light). The second light beam may be incident at an angle of 55° with respect to the normal vector of the sample surface. After absorbing the two coincident light pulses, non-linear effects induced by the non-linear susceptibility of the sample causes the surface of the sample to emit light of a third frequency f3 that is the sum of the first and second frequencies f1, f2 (i.e., an SFG signal).
In one or more embodiments, an SFG spectrum is generated by scanning the first variable frequency f1 across a range of frequencies that span an energy level of a molecular vibrational mode of interest. When the first variable frequency f1 corresponds to the energy level of the molecular vibrational mode, the intensity of the emitted SFG light at the third frequency f3 will increase due to a resonant effect of the first light beam exciting the molecular vibrational mode. By analyzing the intensity of the detected third frequency of light f3, the vibrational modes in the sample may be identified from the resonant frequencies. Furthermore, the directional dependence of the non-linear susceptibility of the sample allows a user to derive information about the orientation of molecules in the sample from the polarization of the collected SFG signal.
In one or more embodiments, the first light beam may be a spectrally broadband light beam that includes a plurality of frequencies f1 while the second light beam remains at a single fixed frequency f2. Accordingly, the emitted SFG light from the sample would include a plurality of third frequencies f3 that may be collected simultaneously for faster data acquisition.
The metal pressure chamber 202 includes a base 208 and a removable lid that enclose the liquid sample holder 204 within the metal pressure chamber 202. The base 208 and the removable lid 210 are formed from a metal and may be aluminum, stainless steel, or any other appropriate metal with sufficient strength to withstand the temperatures and pressures of a simulated reservoir environment. In one or more embodiments, the metal pressure chamber 202 may have a circular cross-section and a diameter of at least 20 cm. Alternatively, the metal pressure chamber may have a rectangular cross-section. However, the metal pressure chamber 202 is not limited to these shapes or dimensions and any appropriate size or shape may be used.
As shown in
A feedthrough 208d may be a channel, a port, a fluid path, a length of tubing, an electrical line, an electrical conduit, an electrical plug, or any combination thereof depending on the material or signal being passed through the base 208. For example, one or more feedthroughs 208d may be electrical conduits that pass signals (e.g., control signals) or power to equipment inside the metal pressure chamber 202, as described below. In addition, one or more feedthroughs 208d may include a channel connected to a chamber pump 230, described below, that pressurizes the interior of the metal pressure chamber 202. Further still, one or more feedthroughs 208d may include various tubes that introduce and remove the liquids sample 206 to and from the interior of the metal pressure chamber 202.
As discussed above, the removable lid 210 cooperates with the base 208 to form the metal pressure chamber 202 that encloses the liquid sample holder 204. The removable lid 210 may be a planar plate that seals against an upper surface of the wall(s) 208b of the base 208. The removable lid 210 may attach to the base 208 by a set of cooperating threads (i.e., screws onto the base 208), one or more clips (i.e., clipped onto the base 208), or by fastening one or more fasteners (e.g., bolts, screws). However, the removable lid 210 may attach to the base 208 by any appropriate means that provides a seal to contain the pressure of the simulated reservoir environment. As shown in
In one or more embodiments, the removable lid 210 comprises a window 214 that allows the liquid sample 206 to be optically accessed from the exterior of the metal pressure chamber 202 (e.g., to allow light from an external source to access the liquid sample 206). The window 214 may be transparent to a first, a second, and a third frequency of light (i.e., frequencies f1, f2, and f3), where the third frequency f3 is the sum of the first and second frequencies f1, f2. The window 214 may be made of glass (e.g., a silica based glass, a calcium fluoride based glass, or the like) that is transparent enough to allow the liquid sample 206 to be illuminated with light of the first and second frequencies f1, f2 from a source disposed outside of the metal pressure chamber 202. The window 214 may also be transparent enough to pass the generated SFG signal comprising light of the third frequency f3 from the liquid sample 206 to a detector disposed outside of the metal pressure chamber 202. The window 214 may have a refractive index of approximately 1.5. The window 214 may be coated with an antireflection coating.
In one or more embodiments, the window 214 may comprise multiple transparent windows. For example, the removable lid 210 may comprise three distinct windows 214, wherein the optical properties (e.g., transmission coefficient) of each window 214 is tuned to a corresponding first, second, and third frequency f1, f2, f3 of light, respectively.
In general, the base 208 and the removable lid 210 cooperate to enclose the liquid sample holder 204 and the window 214 allows external light to access the liquid sample 206. However, other embodiments may be devised without departing from the scope of embodiments disclosed herein. For example, the base 208 may comprise only a base plate 208a while the wall(s) that define the cavity 208c of the metal pressure chamber 202 may be disposed on the removable lid 210. In this configuration, the base 208 may be removable from the lid 210. Accordingly, the one or more feedthroughs 208d may be disposed on the lid 210 rather than the base 208.
As discussed above, the metal pressure chamber 202 encloses a liquid sample holder 204 that retains the liquid sample 206. The liquid sample holder 204 may be made of any appropriate material that retains the liquid sample 206. In one or more embodiments, the liquid sample holder 204 is made of a non-corrosive material (e.g., a stainless steel, a polymer, TEFLON, or the like) that can be easily cleaned of the liquid sample 206 and reused. For example, the liquid sample holder 204 may be made of TEFLON which exhibits excellent chemical and temperature resistance up to 250° C.
The liquid sample holder 204 may be any shape (e.g., circular cross-section, non-circular cross-section) provided that the liquid sample 206 retained by the liquid sample holder 204 is exposed to the interior of the metal pressure chamber 202. In one or more embodiments, the liquid sample holder 204 may be an open cylinder with a circular cross-section and a diameter of 10-15 cm. The liquid sample holder 204 may retain 15-20 mL of the liquid sample 206. However, any appropriate size or shape may be used to retain the liquid sample 206 provided the liquid sample holder 204 fits within the metal pressure chamber 202.
In one or more embodiments, the metal pressure chamber 202 further includes a sample inlet 216 that flows the liquid sample 206 from the exterior of the metal pressure chamber 202 to the liquid sample holder 204 in the interior of the metal pressure chamber 202. The sample inlet 216 may include a sample inlet path 218 connected to the liquid sample holder 204 and a sample pump 220 that pumps the liquid sample 206 through the sample inlet path 218 and into the liquid sample holder 204.
The sample inlet path 218 may be a rigid or flexible tubing that passes through the base 208 via a feedthrough 208d and directly connects to the liquid sample holder 204. The sample inlet path 218 may be disposed to flow the liquid sample 206 directly into the liquid sample holder 204 (e.g., one end of the sample inlet path is directly connected to a wall of the liquid sample holder). In one or more embodiments, the sample inlet path 218 is disposed to flow the liquid sample 206 onto the rock interface 207 disposed in the liquid sample holder 204.
The sample pump 220 may be a metering pump that generates a predetermined flow rate of the liquid sample 206 in the sample inlet path 218. For example, the sample pump 220 may generate a maximum inlet flow rate of 50 mL/min and a minimum inlet flow rate of 0.001 mL/min. However, depending on the reservoir conditions that are being simulated, other flow rates may be used. The sample pump 220 may be a Quizix Q6000 high pressure syringe pump (Chandler Engineering). In one or more embodiments, the sample pump 220 may include a sample storage container or a sample preparation device (e.g., a mixer that combines an organic phase and an aqueous phase to create the liquid sample 206).
In one or more embodiments, the sample inlet 216 may further comprise an inlet valve that seals the sample inlet path 218. The inlet valve may completely seal the sample inlet path 218 to prevent the pressurized environment in the interior of the metal pressure chamber 202 from forcing the liquid sample 206 back into the sample pump 220. Alternatively, the inlet valve may be controlled to partially seal the sample inlet path 218 to regulate the flow rate of the liquid sample 206 from the sample pump 220.
As shown in
The metal pressure chamber 202 further includes a sample outlet 222 that flows the liquid sample 206 from the liquid sample holder 204 in the interior of the metal pressure chamber 202 to the exterior of the metal pressure chamber 202. The sample outlet 222 may include a sample outlet path 224 connected to the liquid sample holder 204 and a sample drain 226 that removes the liquid sample 206 from the metal pressure chamber 202.
The sample outlet path 224 may be a rigid or flexible tubing that passes through the base 208 via a feedthrough 208d and directly connects to the liquid sample holder 204. In one or more embodiments, the sample outlet path 218 may the same type of tubing as the sample inlet path 218.
The sample drain 226 may be a sample storage container or a sample disposal container. In one or more embodiments, the flow in the sample outlet path 224 and out of the sample drain 226 may be passively generated by the sample pump 220 introducing a new portion of the liquid sample 206 into the liquid sample holder 204. Alternatively, the sample drain 226 may also include a pump (e.g., a syringe pump) to actively extract the liquid sample 206 from the metal pressure chamber 202.
In one or more embodiments, the sample drain 226 may further comprise an outlet valve that seals the sample outlet path 224. The outlet valve may completely seal the sample outlet path 224 to prevent the pressurized environment in the interior of the metal pressure chamber 202 from forcing the liquid sample 206 out of the pressure cell. Alternatively, the outlet valve may be controlled to partially seal the sample outlet path 224 to regulate the flow of the liquid sample 206 through the sample drain 226.
The combination of the sample inlet 216 and the sample outlet 222 allows the composition of the liquid sample 206 in the metal pressure chamber 202 to be changed in situ. In other words, the composition of the liquid sample 206 and the liquid/liquid or liquid/solid interfaces found in the liquid sample holder 204 may be actively changed and manipulated to simulate dynamic conditions of the reservoir 102. For example, the liquid sample 206 may be diluted by introducing an aqueous injection solution via the sample inlet 216 to simulate the displacement of an oil/brine sample by conventional water injection recovery techniques.
The pressure cell 200 further includes an ultrasonic stage 228 that is directly connected to the liquid sample holder 204. The ultrasonic stage 228 may be a vibrating table, a vibrating probe, an ultrasonic bath, or any other appropriate mechanism that sonicates the liquid sample 206 in the liquid sample holder 204. In one or more embodiments, the ultrasonic stage 228 may be vibrationally isolated from the metal pressure chamber 202 (e.g., to prevent misalignment of the incident light beams at the surface of the liquid sample 206 or to prevent loosening of the sealed connection between the base 208 and removable lid 210). For example, a thermal isolation layer 240, discussed in further detail below, may absorb mechanical vibrations from the ultrasonic stage 228.
The ultrasonic stage 228 may be connected to a controller 232 that provides power and control signals to the ultrasonic stage 228. The controller 232, described in further detail below with respect to
The pressure cell 200 further includes a chamber pump 230 that is connected to, and pressurizes, the interior of the metal pressure chamber 202. The chamber pump 230 may be a vacuum pump, a compressor, a pneumatic compressor, a hydraulic compressor, any other appropriate mechanism that generates a pressurized environment in the interior of the metal pressure chamber 202, or any combination thereof. In one or more embodiments, the chamber pump 230 may be vibrationally isolated from the metal pressure chamber 202 (e.g., to prevent misalignment of the incident light beams at the surface of the liquid sample 206 or to prevent loosening of the sealed connection between the base 208 and removable lid 210). For example, the feedthrough 208d and/or the tubing that connects the chamber pump 230 and the metal pressure chamber 202 may absorb mechanical vibrations from the chamber pump 230.
The pressure range of the chamber pump 230 may be between ambient atmospheric pressure (e.g., around 14.7 psi) to approximately 3000 psi. However, as conditions in a reservoir 102 (
The chamber pump 230 may be connected to a controller 232 that provides power and control signals to the chamber pump 230. The controller 232, described in further detail below with respect to
The pressure cell 200 further includes a heating stage 238 (e.g., a heating element) that heats the liquid sample 206. In one or more embodiments, the heating stage 238 is an electric heater (e.g., electrical joule heater, ohmic heater), however any appropriate heating element may be used to heat the liquid sample 206. The heating stage 238 may be directly connected to the liquid sample holder 204. In some embodiments, a thermal isolation layer 240 may be disposed on the heating stage 238 (e.g., between the heating stage 238 and the metal pressure chamber 202) to thermally isolate the heating stage 238 from the metal pressure chamber (i.e., prevent the metal pressure chamber 202 from unnecessarily heating during operation). The thermal isolation layer 240 may be made of mica. Alternatively, the thermal insulation layer may a ceramic that includes one or more of aluminum oxide (Al2O3), silica (SiO2), magnesium oxide (MgO), or any combination thereof.
The temperature range of the heating stage 238 may be between 25-100 C.° to simulate the temperatures of the reservoir 102. However, as conditions in a reservoir 102 (
The heating stage 238 may be connected to a temperature controller 242 disposed outside of the metal pressure chamber 202. The temperature controller 242 may be a hardware or software component of the controller 232 or may be a distinct controller apparatus. The temperature controller 242 provides power and control signals to the heating stage 238 through one or more feedthroughs 208d in the metal pressure chamber 202. The temperature controller 242 may control the heating stage 238 based on a temperature of the liquid sample 206 that is measured by a thermocouple 244 connected to the liquid sample holder 204.
In one or more embodiments, the pressure cell 200 further includes a positioning stage 246 that controls a position of a surface of the liquid sample 206. The positioning stage 246 may include one or more actuators (e.g., an electric actuator, a pneumatic actuator, a hydraulic actuator, a piezoelectric actuator, or any combination thereof) that translates the base 208 or the liquid sample holder 204 in one or more dimensions (e.g., a vertical direction) to align the surface of the liquid sample 206 with the incident light beams. The positioning stage 246 may automatically position the surface of the liquid sample 206 based on optical feedback from the surface of the liquid sample 206, as described in further detail below with respect to
In one or more embodiments, the positioning stage 246 may be disposed on an interior surface of base 208, as shown in
In another embodiment, as shown in
The controller 232 may also include one or more input device(s) 408, such as a pressure gauge 234, thermocouple 244, SFG microscope 500 (discussed in further detail with respect to
Further, one or more elements of the controller 232 may be located at a remote location and be connected to the other elements over a network 412. Further, one or more embodiments may be implemented on a distributed system having a plurality of nodes, where each portion of the embodiment may be located on a different node within the distributed system. In one embodiment, the node corresponds to a distinct computing device. In other embodiments, the node may correspond to a computer processor with associated physical memory. In yet other embodiments, the node may correspond to a computer processor or micro-core of a computer processor with shared memory and/or resources.
The SFG microscope 501 includes a first light source 502 that generates light of the first variable frequency f1. The range of the first variable frequency f1 may correspond to the vibrational energy of a molecule in the liquid sample (e.g., corresponds to an infrared wavelength of light). The first light source 502 may be disposed to focus the light of the first variable frequency f1 on the surface of the liquid sample 206 with an incidence angle of 60° with respect to a surface normal vector. In one or more embodiments, the first light source 502 is pulsed laser source with a pulse energy of 2.7-35 mJ and a pulse duration of 28+/−10 picoseconds. For example, the first light source 502 may comprise a PL2231-50 picosecond laser centered at 1064 nm (Ekspla) that feeds into a SFGH500 multichannel beam delivery unit (Ekspla) that feeds a PG501-DFGx optical parametric generator (Ekspla) that outputs a variable IR wavelength ranging of 2300-16000 nm. The first light source may further include a visible laser to aid in focusing the light of the variable frequency f1.
The SFG microscope 501 further includes a second light source 504 that generates light of the second frequency f2. The second frequency f2 is different from the first variable frequency f1 and may correspond to a virtual energy state (e.g., may correspond to a visible wavelength of light). The second light source 504 may be disposed to focus the light of the second frequency f2 on the surface of the liquid sample 206 with an incidence angle of 55° with respect to a surface normal vector. In one or more embodiments, the second light source 504 is pulsed laser source with a pulse energy of 2.7-35 mJ and a pulse duration of 28+/−10 picoseconds. For example, the second light source 502 may be a second output of the PG501-DFGx optical parametric generator (Ekspla) that outputs a fixed 532 nm wavelength.
However, the present disclosure is not limited to this configuration and any appropriate light sources for generating an SFG signal (i.e., light of the third frequency f3 that is the sum of the first and second frequencies f1, f2) may be used. The first and second light sources 502, 504 are configured to spatially and temporally overlap the first and second light beams at the surface of the liquid sample 206 to generate the SFG signal. The SFG signal may be a pulsed signal with a pulse energy of 0.52-5.3 mJ and a pulse duration of 28+/−10 picoseconds.
The SFG microscope 501 further comprises a detector 506 that detects light. The detector 506 is offset from the light sources 502, 504 of the SFG microscope 501 to collect the SFG signal emitted from the liquid sample 206. The detector 506 may include additional optical elements (e.g., lens, spatial filter, frequency filter, spectrometer, power meter) to control, measure, and manipulate the detected light. For example, in one or more embodiments where multiple vibrational frequencies are probed simultaneously, the detector 506 may be a monochromator that collects and spectrally separates different frequencies of light in the collected signal.
In one or more embodiments, the SFG microscope 501 may further include additional optical elements (e.g., mirror, lens, spatial filter, frequency filter, delay line, spectrometer, power meter) to control, measure, and manipulate the emitted and detected light.
In one or more embodiments, the SFG microscope 501 may be controlled by the controller 232. For example, the controller 232 may instruct the SFG microscope 501 to begin data acquisition once the chamber pump 230 has pressurized the metal pressure chamber 202 to a predetermined pressure, the heating stage 238 has heated the liquid sample 206 to a predetermined temperature measured by the thermocouple 228, and the ultrasonic stage 228 has emulsified the liquid sample 206 to a predetermined degree of emulsification.
In one or more embodiments, the controller 232 may halt data acquisition while the sample inlet 216 and sample outlet 222 control the composition of the liquid sample 206 in the liquid sample holder 204. Specifically, adjusting the flow rate of the liquid sample 206 or adding/removing a quantity of the liquid sample 206 may modify the position of the surface of the liquid sample 206 and disrupt the spatial overlap of the first and second light beams at the surface. Furthermore, the controller 232 may halt data acquisition while the liquid sample 206 is being emulsified because the surface of the liquid sample 206, and thus the spatial overlap of the first and second light beams, may be disrupted by the ultrasonic stage 228 process.
Furthermore, the controller 232 may use one or more of the first and second light sources 502, 504 to illuminate the liquid sample 206 to align the liquid sample holder 204 using the positioning stage 246. For example, a portion of the light emitted by the first light source 502 (e.g., the light of the first variable frequency f1 or the visible alignment laser) may reflect off of the surface of the liquid sample 206 and be detected by the detector 506 or a second detector (not shown) of the SFG microscope 501. Alternatively, the detector 506 may detect the SFG signal. Based on a position or an intensity of the detected signal, the controller 232 controls the positioning stage 246 to align the liquid sample 206 with the convergence point of the spatially and temporally overlapped first and second light beams.
At 600, a rock interface 207 is loaded into a liquid sample holder 204 disposed inside of a metal pressure chamber 202 that includes a base 208 and a removable lid 210. The rock interface 207 may be a calcite rock sample or any other appropriate material that may simulate liquid/solid interactions or liquid/solid interfaces that occurring in a reservoir 102 (
At 602, the removable lid 210 is sealed onto the base 208 to seal the liquid sample holder 204 in an interior of the metal pressure chamber 202. The seal may be formed by screwing, clipping, mechanical fastening (e.g., with bolts, screws) the removable lid 210 onto the base 208. However, the removable lid 210 may be sealed to the base 208 by any appropriate means that provides a seal to contain the pressure of the simulated reservoir environment. In one or more embodiments, a seal 212 (e.g., elastomeric O-ring, copper gasket, or other seal) may be disposed between the base 208 and the removable lid 210 to seal the metal pressure chamber 202.
At 604, a liquid sample 206 is flowed from an exterior of the metal pressure chamber 202, through a sample inlet 216, to the liquid sample holder 204. In one or more embodiments, the liquid sample 206 may be a brine comprising a mixture of an aqueous phase and an organic phase that is flowed through a single sample inlet path 218. The flow of the liquid sample 206 in the sample inlet path 218 may be generated by a sample pump 220.
In another embodiment, the aqueous phase and organic phase of the liquid sample 206 may be separate liquids that are flowed into the liquid sample holder 204 by separate sample inlet paths 218a, 218b. The relative proportions of the aqueous and organic phases introduced into the liquid sample holder 204 may be controlled by separate sample pumps 220a, 220b that are connected to the corresponding sample inlet paths 218a, 218b.
At 606, an ultrasonic stage 228 emulsifies the liquid sample 206. In one or more embodiments including a mixture of an aqueous phase and an organic phase (e.g., a brine) as the liquid sample 206, the ultrasonic stage 228 may sonicate the liquid sample 206 to emulsify the two phases.
At 608, a heating stage 238 heats the liquid sample 206 to a simulated reservoir temperature. In one or more embodiments, the temperature of the liquid sample 206 is raised to approximately 90-100 C°. However, as discussed above, the present disclosure is not limited to this temperature range because conditions of a reservoir 102 may vary according to many parameters (e.g., depth, geographic location, rock composition). The temperature of the liquid sample 206 may be monitored by a thermocouple 244 that is connected to the liquid sample holder 204. The thermocouple 244 may send temperature information to a temperature controller 242, or alternatively a controller 232, that sends power and control signals to the heating stage 238.
At 610, a chamber pump 230 connected to the interior of the metal pressure chamber 202 increases the pressure inside the metal pressure chamber 202 to a simulated reservoir pressure. In one or more embodiments, the pressure of the liquid sample 206 is raised to approximately 3000 psi. However, as discussed above, the present disclosure is not limited to this approximate pressure value because conditions of a reservoir 102 may vary according to many parameters (e.g., depth, geographic location, rock composition). The pressure of the interior of the metal pressure chamber 202 may be monitored by a pressure gauge 234. The pressure gauge 234 may send pressure information to the controller 232 that sends power and control signals to the chamber pump 230. Furthermore, the controller 232 may control a control valve 236 to seal the metal pressure chamber 202 from the chamber pump 230 or release pressure from the interior of the metal pressure chamber 202.
At 612, a surface of the liquid sample 206 is illuminated with light of a first variable frequency f1 and light of a second frequency f2 through a window 214 of the metal pressure chamber 202. The incident light beams of the first and second frequencies f1, f2 are spatially and temporally overlapped at the surface of the liquid sample 206 to generate an SFG signal (i.e., light of the third frequency f3 that is the sum of the first and second frequencies f1, f2).
In one or more embodiments, a positioning stage 246 may translate the surface of the liquid sample 206 to align the surface of the liquid sample 206 with the incident first and second light beams. The positioning stage 246 may automatically position the surface of the liquid sample 206 based on a reflected signal from the surface of the liquid sample 206 (e.g., alignment with the surface of the liquid sample 206 is achieved when the reflected signal exceeds a predetermined threshold or reaches a predetermined position on a detector 506). Alternatively, the positioning stage 246 may automatically position the surface of the liquid sample 206 based on an intensity of the generated SFG signal (e.g., alignment with the surface of the liquid sample 206 is achieved when the SFG signal is maximized or exceeds a predetermined threshold). In yet another embodiment, the positioning stage 246 may be controlled manually.
At 614, the SFG signal comprising light of a third frequency f3 is collected from the surface of the liquid sample 206 for analysis.
At 616, the liquid sample 206 is flowed from the liquid sample holder 204, through a sample outlet 222, to the exterior of the metal pressure chamber 202. In one or more embodiments, the liquid sample 206 that is removed from the metal pressure chamber may be replace by a new liquid sample 206 from the sample inlet path 218.
In other words, in one or more embodiments, the composition of the liquid sample 206 may be altered in situ by flowing different solutions or different proportions of the aqueous phase and organic phase into the liquid sample holder 204 and removing the liquid sample 206 that has already been studied. Thus, the liquid sample 206 may be characterized in both static and dynamic reservoir compositions (e.g., stable live oil compositions or dynamically changing compositions that may model displacement of hydrocarbons by an injection fluid).
In one or more embodiments, In one or more embodiments, the heating stage 238 and the chamber pump 230 may dynamically change the temperature and pressure inside the metal pressure chamber 202 during acquisition of the SFG signal. For example, the controller 232 may ramp the temperature or pressure to different values in response to data collected from the pressure gauge 234, the control valve 236, the thermocouple 244, the detector 706, or any combination thereof. Thus, the liquid sample 206 may be characterized in both static and dynamic reservoir environments (e.g., stable temperature and pressure conditions or dynamically changing temperature and/or pressure conditions).
In one or more embodiments, the first variable frequency f1 may be continuously or discretely changed to obtain a spectrum of SFG signals from the liquid sample 206. In another embodiment, first variable frequency f1 may be a spectrally broadband frequency range that includes a plurality of frequencies. Accordingly, a spectrum of SFG signals from the liquid sample 206 may be obtain at one time.
Software instructions in the form of computer readable program code to perform embodiments of the present disclosure may be stored, in whole or in part, temporarily or permanently, on a non-transitory computer readable medium such as a CD, DVD, storage device, a diskette, a tape, flash memory, physical memory, or any other computer readable storage medium. Specifically, the software instructions may correspond to computer readable program code that when executed by a processor(s), is configured to perform embodiments disclosed herein.
One or more of the embodiments disclosed herein may have one or more of the following advantages and improvements over conventional SFG spectroscopy techniques: simulating reservoir conditions (e.g., high pressure, high temperature environments); simulating reservoir interactions for study in a controlled environment; SFG spectroscopy under static and dynamic temperature and/or pressure conditions; SFG spectroscopy with dynamic sample compositions to analyze more accurate liquid/liquid and liquid/solid interfaces that occur in hydrocarbon reservoirs. One or more of the above advantages may improve a user's understanding of the chemical and molecular structures and interfaces that occur in a reservoir and improve the effectiveness of hydrocarbon recovery techniques.
Although the disclosure has been described with respect to only a limited number of embodiments, those skilled in the art, having benefit of this disclosure, will appreciate that various other embodiments may be devised without departing from the scope of the present disclosure. Accordingly, the scope of the disclosure should be limited only by the attached claims.
| Number | Name | Date | Kind |
|---|---|---|---|
| 20180180404 | Hunt | Jun 2018 | A1 |
| Number | Date | Country |
|---|---|---|
| 110132789 | Aug 2019 | CN |
| 111213633 | Jun 2020 | CN |
| 2004111444 | Apr 2004 | JP |
| Entry |
|---|
| Non-Final Office Action issued in related U.S. Appl. No. 16/787,849, dated Jul. 26, 2022 (8 pages). |
| Number | Date | Country | |
|---|---|---|---|
| 20220221440 A1 | Jul 2022 | US |
| Number | Date | Country | |
|---|---|---|---|
| Parent | 16787934 | Feb 2020 | US |
| Child | 17710374 | US |
