SA520420923B1 - Systems and Methods for Tri-Axial NMR Testing - Google Patents

Abstract

Systems and methods for testing properties of a test sample with a tri-axial nuclear magnetic resonance apparatus (100) include a tri-axial load frame (110) encasing a tri-axial load cell (120) having a tri-axial sample holder (150) and a piston assembly (206). A radial space (190) surrounds the tri-axial sample holder (150). The tri-axial load frame (110) further encases at least one end cap (180) operable to contact the tri-axial load cell (120), and a nuclear magnetic resonance instrument (170). An axial pressure line (220) is in fluid communication with the piston assembly (206), a confining pressure line (214) is in fluid communication with the radial space (190), and a pore pressure line (216) in fluid communication with the test sample. The axial pressure line (202), the confining pressure line (214), and the pore pressure line (216) are independent and separate fluid flow paths. Fig. 1

Description

Systems and Methods for Tri-Axial NMR Testing Full Description General background of the invention; This disclosure relates to a nuclear magnetic resonance (SDE) SDE (NMR) resonance test of 11-2"18 axes by a triaxial nuclear magnetic resonance (NMR) NMR tester. The 101/14 nuclear magnetic resonance tester is triaxial Capable of evaluating the properties of different sample materials under Oba temperature and pressure conditions.In the hydrocrion industry it is important to evaluate the fluid-solid interactions at the blister bed at formation temperature and pressure conditions.When reservoir fluids are produced, the temperature, pressure, and The fluid phase “fluid composition” and rock behavior are constantly due to changes in temperature, pressure, and other variables.These changes can be modeled so that their effect on reservoir production can be explained.ill hole cementation is critical processes during jee blistering.Cementation does not affect affect not only the production process, but also lead to environmental problems related to gas migration and pollution of aquifers, and affect the stability of the blistering pit.The cement pumped into the fy pit undergoes a pumping cycle; For cementation mission 5 successful. The subterranean formation may have millions of years for the temperature to stabilize; pressures and fluid flow. The cement used in a blister pit must withstand the same tank conditions as the formation itself. Cement used in a blister pit must be evaluated under the same tank conditions that the cement will encounter Other fluids used during various hydrocarbon development processes such as pall 0 and completion; interference; and perforating fluids at reservoir temperature and pressure conditions. For example » lead

The fluids used during drilling operations are many (Jie algal) to lubricate the bit and maintain a temperature

the heat of the bit and the iad tubing string) and provide a load on the bit so that the bit is pushed

in the rock; providing pressure in the dl bore to mitigate any backflow or explosion of the reservoir fluids;

And push the bridging material to penetrate the pores inside the rock in the blister hole that is drilled and sealed. It is important to understand how these fluids operate under tank conditions.

General description of the invention

These detection forms can provide test results based on data collected from samples

extracted from the pulp; cutting; and payments »; cement; and fluids in the tank. Systems and methods include this

Detection Collect data on samples that are exposed to pressures and temperatures of the bottom of the well. systems lack

0 and current NMR test sample methods indicate the ability for Jie to generate this data under reservoir conditions. The data collected can be linked to a broader set of data that is continually obtained during enrollment; Well testing and seismic data collection. in the form for this disclosure; A three-axis NMR apparatus for testing the properties of a test specimen comprises a three-axis bearing frame enclosing a three-axis bearing cell and a piston assembly.

5 The triaxial load cell contains the triaxial sample dels and defines the diagonal space surrounding the triaxial sample holder. The triaxial load frame encapsulates at least one operable end cap to contact the triaxial load cell and the NMR instrument. An axial pressure line is in fluid contact with the piston assembly. The bound pressure line is in contact by means of a fluid with the radial space. The pore pressure line is in contact with a fluid with a sample

0 _ test. The axial pressure line is considered; restricted pressure line; And the pore pressure line is independent and separate fluid flow paths. in alternative models; Restricted pressure line can extend; and a porous pressure line through at least one end cap. At least one terminal cover may contain an operable conductor for the flow of electric current. At least one end cap can locate one or more cavities to house

At least one acoustic sensor. The device can be operable to maintain an axial pressure greater than constrictive pressure and greater than pore pressure. The test sample can be a fluid; or cement; or cut pits or cores of a coal bed methane tank. in an alternative form to this disclosure; The method for using the 5-axis EN NMR machine involves obtaining the test sample and loading the test sample into the 3-axis sample test stand. The 3-axle sample holder is loaded into a 3-axle load cell to create a 3-axle loaded load cell. Axial pressure is applied by providing an axial pressure fluid through the axial pressure line. A confining pressure is applied by supplying the confining pressure fluid through the cial pressure line and the confining pressure is less than and independent of the axial pressure. The 0 temperature control fluid can be rotated around the three-axis sample holder by supplying the temperature control fluid through the temperature control flow line. The data is measured from an NMR machine. In alternative embodiments the Wail method may involve the application of pore pressure by supplying the pore pressure fluid through the pore pressure line; where the pore pressure is less than and independent of the axial pressure and the constraining pressure. The axial pressure can be in the axial pressure range from 6.89 kPa to 3,450,000 kPa; The bound pressure can be in the bound pressure range of 6.89 kPa to 214,000 kPa and the pore pressure can be in the pore pressure range of 6.89 kPa to 207,000 kPa. in other alternative models; The method may also include measurement data from at least one acoustic sensor 0 and at least one electrical sensor. Sa due the test being blister-pit cement Say the method also includes shal tests on the blister-pit cement. The test sample can be drill bits and the method can also include tests on Drilling cuttings The test sample can be core from a coal bed methane tank and the method can also include tests on core from a coal bed methane tank.

A Brief Explanation of the Drawings Now that the way in which the features will be rendered has been verified; Aspects and advantages of detection models as well as others (Sag) can be understood in more detail; a more brief description of detection alae can be given in this disclosure by reference to the models which are illustrated in the drawing which forms part of this specification 0 and yet It should be noted that the attached drawing shows only certain z models for detection and should not be used

Consider it ike for the extent of detection; Where detection can allow other equally effective models to be included. Figure 1 is a three-axis NMR device ly of a detection model. Detailed Description: Although the following detailed description contains specific details for the purpose of clarity; he will realize

0 Many with regular skill in the field Many examples are included; Variations and alterations in the following descriptions are within the scope of disclosure. apply on it; The forms described in this list and in the attached figure are mentioned without any prejudice to the circular. land (ang) is not required on protected models. Detection is generally related to cll analysis and fluid analysis; and petrophysical analysis and evaluation of phase behavior

5 1 for hydrocarbon tanks under conditions of triaxial stress with pore pressure. The three-axis NMR apparatus described here performs multiple tests on Le at the same time and also integrates the collected data related to the different properties of the sample. The device allows tank modeling. For example » when collecting audio data; Jie audio data; during resonance measurements

0 Nuclear Magnetic Levitation (NMR) instrument will provide information regarding changes of mechanical stress on the sample not only as a function of pressure change; but Load with formation fluid changes. This information is directly used during seismic monitoring of reservoir production and to adjust simulation models for production profiles.

on one side; The detection provides a triaxial NMR device for testing petrophysical properties and collecting geomechanical information. The triaxial NMR apparatus comprises a three-axial load frame enclosing a three-axis load cell with a three-axial sample holder and a diagonal space surrounding the three-axial sample holder. At least one end cap can be operated to contact the three-axis load cell. The device also includes one electrical sensor on “JY” and at least one acoustic sensor; and a nuclear magnetic resonance instrument. The three-axis load cell includes the three-axis sample holder. The triaxial specimen stand may be made from any material acceptable for the triaxial specimen stand. in general; The triaxial sample holder will not have an NMR signature or a known NMR signature. in certain models; The triaxial 0 sample holder is made of TORLON® (available from Solvay Plastics) TORLON® has a sufficient pressure and temperature rating and is “invisible” to NMR The triaxial sample holder can be designed so that it does not 5 (ging) holes for fluid or electrical connection on the outer surface. In some embodiments, the design of the three-axis specimen holder is such that the three-axis specimen holder (BIA) is free of any contact on the outer face of the three-axis specimen holder. This design provides collar strength Greater for greater constraining pressures.This design has the added benefit of reducing the wall thickness of the LER vessel) allowing the use of a larger diameter sample.In some embodiments the triaxial sample holder is in the shape of a cylinder.In other embodiments the cylinder diameter can range from about 2.5 millimeters (mm) to about 102 mm.0 roll length can range from about 2.5 mm to about 508 mm.In general, the triaxial sample holder is able to withstand the level of stresses associated with generating cracks in the tank and is capable of applying axial stress equal to the pressures in the tanks.Triaxial load cell can provide axial pressure independent of constraining pressure and pore pressure. The triaxial load cell is connected to a pump and pressure gauge to apply and control the axial pressure 5 on the sample loaded in the Jala Triaxial Specimen. Triple load cell can be used

Axons for initiating cracks in a sample to study crack mechanics with fluid transport. in some embodiments; The triaxial load cell is made of titanium coated. The triaxial load cell also includes pore pressure lines; acoustic sensor feeders; and electrical sensor feeders. pore pressure lines can be applied; and feeders

acoustic sensors; and electrical sensor feeders on or in the end caps. Fluid is supplied for both constraining pressure and pore pressure through at least one end cap on the three-axle load cell. in some embodiments; There are two end caps. The end caps can be floating end caps that can accommodate different lengths of specimens within the same three-axis specimen holder.

0 end caps can accommodate pressure lines to allow fluid flow. Pressure lines allow fluid to flow into the radial space surrounding the triaxial sample holder; to the triaxial sample holder; and in the piston assembly. Fluid flow can be provided through pressure lines using syringes; or application; Or any other supply mechanism known to those skilled in the art. On some oz dails the end caps have three pressure lines. In some eg mail the covers are

5 terminal made of aluminum or TORLON® in other models; The end caps are enclosed with a connector that allows electrical current to flow. Any acceptable connector can be used. in certain models; The connector is chosen from gold; Or platinum, or aluminium. Wad end caps have one or more recesses to house at least one acoustic sensor.

0 A three-axis load frame encapsulates the components of the device. in general; The 3-axle load frame must not have an NMR signature or a known NMR signature. in some embodiments; The 3-axis bearing frame is constructed of titanium with an additional coating to increase NMR inertia and handle corrosive chemicals; acids; and industrial solvents that may be used during the test. These chemicals include toluene, methanol, and chloroform; and dioxide

the creon is in the liquid state; or invasive; or liquid and gaseous; methane; water; zeppelin” and hydrochloric acid; and acetic acid. in other models; The triaxial load frame can be expanded to accommodate longer samples. in some embodiments; The 3-axle load frame Beal Lal encapsulates deformation measurement such as linear variable differential transducer and strain gauge; An infrared or acoustic displacement system for measuring the static mechanical properties of a sample. In other models, the three-axle load cell is equipped with a piston separator for different pressure, volume and temperature analyses; jie viscosity; compression; fixed installation stretch; wax; asphalt; formation of hydrates. in one of the models; If the sample is a fluid and a specific NMR probe is used; It is possible to detect asphaltene as a function of Creon-13. It is also possible to determine the structure of 0 hydrate; It is a desirable aspect for hydrate production and to ensure a dilute flow; In addition to wellbore stability issues related to wax; asphalt; and hydrate; and crystallize the salt. in some embodiments; At least one electrical sensor is a resistance probe that provides measurements of electrical properties at the same time as other properties. This helps in the integration of various laboratory and field data for both rocks and fluids in the reservoir. in some 5 models; The fluid and its associated pore line on the tips of the Jala sample triaxial can be used to measure the electrical response. in cases of non-conductive fluid; Non-magnetic conductors may be attached to the sample during sample preparation for the purpose of electrical properties measurements. in some embodiments; An impedance analyzer can be used to evaluate voltage; current, phase, and resistance of the sample. in some embodiments; The acoustic sensor is an acoustic transducer with variable frequency and mode; Jie 0 cut and longitudinal. Different position transducers allow; together with the variable frequency; analyzed to target the specific pore size; or particle size; or fluid components. The acoustic transducer measures various dynamic properties of a sample under triaxial conditions with accurate fluid saturation and an easy path to log data integration. in some embodiments; At least one acoustic sensor shall be operable to act as a transmitter and receiver. Among the acoustic properties that can be measured 5 include the P wave, which is longitudinal; wave 5; They cut at angles of 180 and 90; and 45 degrees in each

transmission and reflection mode; travel time along with the entire frequency spectrum. Dual-mode transducers can be selected based on sample size and test procedure” with frequency ranges from the number of kilohertz (KHZ) used in massif and fluid properties recorders to larger frequency ranges for checking detailed diffusion patterns and pore geometry with test samples . Many of these transducers are readily available. in addition to; Waal skilled in the art can custom design a transducer based on specific sample variables under verification. With the ability to perform acoustic measurements in different positions using the 3-axis 11414 device, there is a growing understanding of formation damage due to sand migration; And formation damage due to leakage of wax and asphaltine with changes in temperature and pressure. These measurements will also help evaluate the interaction of the fluid 0 presented with the rock matrix; Especially in chemical enhanced oil recovery (EOR) where triaxial power helps simulate a system stress in a given reservoir more than conventional hydrostatic test vessels currently available. Additional Load volume and resistance measurements provide a convenient way to calibrate field log data prior to EOR is domain specific. Any NMR instrument can be suitable for these particular applications. In general, large-hole NMR with adequate signal-to-noise ratio, and signals received with minimal time delay, are acceptable. In general, the NMR should have the appropriate gradient and hole diameter for the triaxial load cell.The NMR with appropriate combination of gradient and low time delay will not only provide the saturation profile between hydrocarbon and non-hydrocarbon fluids, but will also determine the associated water and heat and will help distinguish between oil and kerogen and may help distinguish between 0 hydrocarbon gases kerogen and asphalt NMR can have the ability to perform whole and thin slice scanning The ability to perform focused NMR scanning on a smaller area will offer advantages More detailed sample. This technique can be used to measure the permeability of an unconventional airtight reservoir and will be able to distinguish between the matrix permeability and the crack permeability; and the spread of different fluids. A fluid will be provided on one side of sample 5 and the 0/14 will be swabbed! Time-dependent slide to know the movement and shape of the anterior part of what

It provides a valuable transfer behavior for the reservoir sample. in some embodiments; A three-axis NMR device will be equipped

GPS controlled device; or a cell packing device to provide accurate and reproducible slice location.

This can be achieved for a shorter sample by moving a window between the NMR bore hole and the test vessels

For a longer sample, the NMR can be fully packaged to provide slide scanning. The NMR machine is capable of performing NMR scans from 0.1 mm to 152.4 mm slice; at a rate of 360 degrees.

in addition to; NMR can have a variable magnetic field and frequency ranging from a number of

kilohertz to a number of megahertz (MHZ) This range will help focus on various components

Rocks and fluids in detail.

The Lad NMR could contain a variable probe for hydrogen and carbon-13; sodium;

0 and components (AY) that are likely to be in a tank. This probe will focus the test on different components of the rock texture and fluids. For example (JE) the sodium probe scan along with the hydrogen probe probe will amplify the difference between free water and bound water” as well as provide information about the salinity of the formation. cially the carbon-13 probe can help determine the maturity and type of kerogen in a sample.

5 in other models; The triaxial NMR device has a pore pressure capability that allows the fluid pressure to be raised to reservoir conditions. in addition to; This setup allows the measurement of permeability in both the steady state and the unsteady state with either dead or live fluids. Steady-state is a relative permeability test in which two or more fluids are simultaneously supplied at one end of a cylindrical plug sample of reservoir rock and the change in sample fluid saturation is monitored as a function of the fluid produced over

0 the other end to simulate tank injection. An unsteady state is a test in which one fluid is supplied into a rock cap sample in the presence of a second fluid within the sample and the production of both fluids is monitored at the other end of the sample. This simulates how the tanks are initially formed and is also the primary oil production mechanism. A dead fluid is a fluid that does not contain gas or has very little ALE of it. A Ble all fluid is a fluid in which a gas has a breath

5 The chemical composition present in a particular hydrocarbon reservoir.

— 1 1 — in other embodiments; The triaxial NMR apparatus can also include one or more semi-permeable membranes for analysis of capillary pressure and wettability measurements. In one of the designs for setting up the tool; One or more porous semi-permeable membranes can be combined to perform analysis of capillary pressure and wettability of a reservoir sample under triaxial test conditions with saturation NMR and other measurements. There are many advantages to Jie performing this analysis” beyond its use of data integration. Jian One of the main advantages of this analysis is the tuning of the different empirical equations used to simulate reservoirs with real data. in other models; The Wad can include a feed to a second NMR for injection and evaluation of the production fluid under stress conditions. This added a value of 0 to perform a detailed search to evaluate different nanotechnology fluids and other phase behavior attributes of the reservoir or injected fluids. on the temperature during testing with a temperature controlled fluid. The 3-axis NMR Wad includes pumps to provide 5 different sample pressures and fluid flows. In some oz all b the triaxial NMR federated resonance apparatus includes a sample strain-measuring system or a displacement-measuring apparatus. The sample strain measurement system or displacement measuring instrument can be electric, infrared, acoustic or any other type based on dual and test condition requirements. The advantage of performing stress measurements on die reservoir rock is that they relate to 0 mechanical strength and formation damage issues. The advantage of performing stress measurements on a fluid sample is that it relates to production profiles and flow assurance issues. The triaxial NMR apparatus can also incorporate an appropriate density meter and viscometer at the injection and production ends to assess transfer behavior. These types of gauges provide valuable information about changing fluid properties during testing of a core sample. For example; These may appear

— 1 2 —

Tests it at different pressures and flow rates; The possibility of emulsification of the injected fluid and rock matrix. in other models; The 3-axis NMR apparatus incorporates an acoustic barrier on the production end for production measurements. Acoustic barriers are known by people skilled in

the field. Such people can easily select a suitable sound barrier for use in this disclosure. in other models; The three-axis NMR apparatus includes an oscillating fluid injection system and a cylinder for injecting live fluids. Fluid swing injection systems and cylinders are known to people skilled in this field. Such people can choose suitable cylinder and injection systems

0 fluid flip-flops for use in this disclosure. In gil models the triaxial NMR system includes pressure sensors sensitive to various sample and fluid pressure monitoring. Sensitive pressure sensors are known to persons skilled in the art. Such persons can easily select a suitable pressure sensitive sensor for use in this detection.

5 shows a triaxial NMR device 100 according to a detection model. This model of the device contains a three-axle load cell 110. The device also includes a three-axle load cell 120; NMR device 70 1, end caps 1 80, acoustic sensors 1 30, electrosensors 0. Triaxial sample holder 150) and pressure lines 200; conductors 212” and bore (Glad 0). Insulation sleeve 160 can be added to enclose the triaxial sample holder. In addition

0 so; Shown is a 190° diagonal space surrounding the triaxial sample holder. The acoustic sensors are spaced 130° and the electrical sensors 140° away from the sample so that the NMR instrument has an unobstructed view of the sample. In an example of operation, the method for using the 3-axis NMR apparatus includes obtaining the lial sample and loading the test due into the 3-axis sample holder; and download

Triaxial sample holder in a three-axis load cell to create a three-axis loaded load cell. if the sample is a solid sample Jie pulp sample; or cut off; or earplugs; or cement sample; The sample can be loaded into the triaxial load cell as an intact sample that has not been crushed. after crushing the sample; The sample can no longer be re-pressurized to tank conditions. in addition to; 5.For applying restricted stress to a rigid die; The specimen must have a definite circumference and to apply an axial load to a solid specimen; The sample should have a flat ple-shaped terminal surface. The loaded triaxial load cell is then placed in contact with at least one terminal cap of the triaxial NMR device. A triaxial pressure is then applied to the triaxial load cell. Triaxial pressing can include axial pressing and 0 bound pressing. in certain models; Triaxial pressure can also include pore pressure. in order to apply axial pressure; An axial pressure fluid is applied via the axial pressure line 202 and in the piston Ban 204. The piston chamber 204 is gin of the piston assembly 6. The piston assembly 206 comprises the piston member 208 which is connected to a structural member of the three-axle bearing frame 110. The chamber connects The piston 204 with the end cap 180. When the axial pressure fluid is transferred to the piston chamber 204; The end cap 204 is pushed axially 180 away from the piston member 208 so that the end cap 180 applies axial pressure on the sample. in order to apply constraining pressure; A restrictive pressure is wile applied through the single end cap on the JY by means of the restrictive pressure line 214 and into the diagonal space 190 that skirts the sides of the sample to apply a restrictive pressure to the sample. for applying pore pressure; A pore pressure fluid 0 is applied through one end cap to the JV via the pore pressure line 216 and in contact with the sample to apply pore pressure to the sample. The axial pressure line is considered; restricted pressure line; And the pore pressure line is independent and separate fluid flow paths. alternatively The test due can be a fluid or a fluid containing some solid or gas such as cement slurry; or drilling fluids or reservoir fluids” or chemicals for 5 508. In Jie this form; The test fluid sample can be injected through the pore pressure line

6 and in a three-axis sample holder. When the test fluid die is inserted into the sample holder

triaxial; One or more end caps are pushed 180 in away from the end

the other for the end caps so that the fluid sample to be tested is placed inside the sample tripod

interlocutor. After the fluid sample to be tested has been placed inside the triaxial sample holder; The pressure of the fluid sample is maintained at a pressure lower than the axial pressure and the constraining pressure.

The flow path of the axial pressure fluid is separate and independent from the flow path of the limiting pressure fluid

And separate and independent of the flow path of the pore pressure fluid. Axial pressure is applied uniformly

Independent of constraining pressure and pore pressure. likewise; The limiting pressure fluid shall be separate and independent

About the flow path of the pore pressure fluid.

0 while the triaxial NMR device is operating 100; Axial pressure is applied and maintained at a larger amount than the limiting pressure. when there is pore pressure; Axial pressure is applied and maintained at a greater amount than the pore pressure. thanks to the ability to independently adjust the axial pressure; The constrained pressure and pore pressure allow simulation of real triaxial stress conditions observed in hydrocrion tanks. The independent axial stress is greater than the stress

5 constraint is responsible for changes in the structure of the pore throat that control fluid motion in actual aquifers. In BAD the rocks and fluids are under triaxial conditions where the axial pressure is greater than the bound pressure and the pore pressure; and the pore pressure is less than the bound pressure. If the pore pressure is greater than the bound pressure the reservoir will crack and fail. Only by repeating these conditions Dual) can be tested at repeated blister bottom pressures.

Sa 0 then rotate the temperature control fluid around the loaded three-axial sample Jala by supplying the temperature control fluid through at least one end cap into the diagonal space surrounding the three-axial sample holder. The temperature control fluid can be connected via the temperature control flow line 210 to maintain the temperature of the triaxial sample holder during analysis. A test fluid can then be supplied to the loaded triaxial sample holder from

25 through at least one end cap by means of pressure lines. shal is cleared by ringing

Time-dependent slice NMR of the sample using the NMR instrument. Electrolysis of the sample using at least one electroacoustic sensor and acoustic analysis of the sample using at least one acoustic sensor are also performed. Samples can be obtained from any reservoir. Reservoirs from which the sample may be obtained include non-residual reservoirs; such as shale gas; gas sands (Gall and heavy oil), tar sands; hydrates; and beneficiary EOR reservoirs. The samples used for analysis can be an original sample or a clean sample. The term original sample means a reservoir cap sample that has been drilled and retrieved from the reservoir and mounted in a sample tripod axes without any rotation A clean sample means a sample that has passed 0 after its retrieval from a tank by various processes to remove all fluids and associated solids such as salt, wax, and asphalten Triaxial pressures can include any combination of the following pressures: axial pressure; confining pressure; The pore pressure of the sample is at least about 100 psi lower than the constraining and axial pressures.In general, the pressures are chosen to simulate the conditions of the reservoir under study.During the analysis Jala can control the temperature of the sample triaxially to simulate the conditions of the reservoir under study. In some embodiments, the temperature can be controlled using a temperature control fluid. 0 Acceptable temperature control fluids include any known temperature control fluids that have little or no known effect on the NMR resonance signal in some embodiments; The triaxial sample holder is kept at a temperature between about -20 °C (p°) and 350 °C. In general; the temperature is sly chosen on the temperature conditions in the tank or other material under study.

The test fluid supplied to the three-axle specimen holder loaded through at least one end cap comprises a variety of fluids. a3 indicates that the test fluid has been injected; or put it; or otherwise supplied to the sample Jala triaxial. For example; Solvents such as toluene, methanol, and chloroform can be provided; xylene” and water; and dioxide

Carbon to wash lin Kgl and salts. Acids can be supplied in different concentrations for cleaning and simulation processes. (Sar) Provide hydrocarbon liquids, gases, and brines for flow capacity measurement. Wettable EOR chemicals can be provided for simulations. Fracture fluids using props can be provided for simulations. In some embodiments, the test fluid is a dead fluid. In other embodiments, the test fluid is a live fluid.

0 in some models; A time-dependent slice NMR scan of the sample measures NMR frequencies from about 0.1 kHz to 20 MHz. The frequency will be chosen based on the type of sample being evaluated and the variables under study. For example; For a homogeneous sample of the single pore type with a fluid having a viscosity in the range of 0.5 to 2.0 cPa (60); An NMF of 2MHz may be acceptable. However; for the fluid

5 most viscous with heterogeneous rock pore system with multiple pore type; A combination of 2MHz and 12MHz may be required for the nuclear magnetic frequencies. in other models»; The NMR instrument was equipped with variable probes to perform analysis on the samples. Acoustic analysis of the sample measures frequencies from about 1 Hertz (Hz) to 100,000MHz. Sample size may dictate frequency. For example; For a medium-sized sample; The range may range between

0 500 kHz to 1 MHz. For smaller sample clans a frequency greater than 1MHz may be necessary. Larger sample sizes may require lenses less than 500MHz. The different models for this detection will reduce the time it takes to assess the tank. By running multiple analyzes together there will be significant time-saving operational benefits. in addition to; Data accuracy will be improved and integration with field and record data will be improved. Will provide current disclosure forms

5 Comprehensive study platform for EOR and shale gas analysis.

— 7 1 — A triaxial NMR instrument is capable of performing a number of different tests. Among the tests that can be performed are: cond NMR testing under triaxial conditions with no pore pressure; NMR test under triaxial conditions with pore pressure; NMR test under hydrostatic conditions with or without pore pressure; NMR test) with a combination of three axes; hydrostatic cae changed electrical “acoustic” pore pressure; Temperature;

Slide “JE NMR (NMR deformation measurement) stress changes (axial ¢ constrained porosity) fluids (acoustics; density; electrical measurements) fluids (pressure, volume, temperature” and flow rate and component measurements (in-flow and out-flow)); NMR with mechanical tests and sensor array; NMR tests with steady-state permeability test; triplicate conditions

0 axes and sensors for various petrophysical and geomechanical data; NMR tests with unsteady state permeability test; triaxial conditions and sensors for various petrophysical and geomechanical data; NMR tests with laminar capillary (membrane) pressure test; triaxial conditions and sensors for various petrophysical and geomechanical data; 11l ¢EOR and Gravity Drainage Assisted Steam and Gas Substitution Tests for Water; lg oxide

5 carbon»; chemicals » and surfactants; steam and acid treatments; NMR tests on fluids such as heavy bitumen; and hydrate; quantities of asphalt; crystallization under hydrostatic conditions; NMR tests with pressure, volume and temperature (constant expansion of the structure; differential release); and flow assurance studies under hydrostatic conditions. An example test procedure is described as follows:

0 Prepare the 3-axis NMR machine and perform system calibrations. Prepare test samples. Prepare the NMR instrument setup based on the test and sample type; Such as whether the sample is from a core material or a fluid sample. Prepare the correct N M R probe and perform base calibrations.

— 8 1 — Install the sample in the 3-axis sample stand. Install the 3-axis sample holder into the 3-axis load cell. Install the 3-axis load cell into the NMR device using the terminal caps and connect all the feeds to the fluids and data sensors. Apply an initial axial pressure of about 50 psi. However; This step can be modified based on the elastic properties. For example (Jad) endodontic specimens may be scanned with a CT scan to indicate whether the specimen is soft or filamentous. For stronger samples; The initial pressure may start at 1000 psi or more. Fix the axial displacement and increase the constraining pressure and pore pressure on the sample until the sample reaches the test pressures. This step can be modified based on the sample used and the test procedures required. Rotate the temperature control fluid around the triaxial sample holder and monitor the sample temperature and pressure along with other data such as acoustic information and stress resistance. Once the sample has reached the test conditions (glad) and all test variables are in a pseudo-equilibrium position as the accepted fluctuations based on specific test variables; Never test. 5 During the test » monitor all sensors; pressures; test variables for measuring and collecting acoustic data”; electrical, NMR and other data. Run tests on the test sample and collect data from the sensors. Analyze the data collected. Cling the samples and reduce the temperature to ambient or close to 0° ambient temperatures and then reduce the various pressures in such a way as to maintain the integrity of the sample. In an example of the process; The sample can be Ble for drilling bits. during field operations; Drill bits are continuously produced and sent to the mud pit where the field engineer can look at them

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Visually for evidence of hydrocorion. Drill bits have a wealth of information within them that is greatly increased in value when the chunks are analyzed soon after they reach the surface. for example; One of the most important variables for evaluating the size of a hydrocarbon discovery is the amount of hydrocarbon lie in non-hydrocarbon fluids; such as cellal).

Over time, the pieces dry out, fluids are lost, or the porous structure of the pieces is rearranged. The value of data collected from plots decreases dramatically over time and can provide incorrect results if too much time passes before the plot is evaluated. When these pieces or when the pulp reaches the laboratory in a matter of hours; or all or weeks of aig analyzed by Bae times after months” lose the quality of the data. Triaxial NMR lea can be used for this on-site detection and rapidly applying tank pressures to

0 -_ field seals or sale cutting samples Samples to reservoir conditions and measurements can be made to provide data on fluid types, fluid saturation, fluid location and electrical response; Voice response and other collections of valuable data in a timely manner. In an alternative example of a process, the sample could be the core or pieces of a coal bed methane tank. The current practice for testing samples from a coal bed methane tank involves two steps

5 separate tests using two separate tools. The first test involves cutting a core out of the material and keeping the core underwater in test vessels under ambient pressure for several months to estimate the gas rating. The second test involves cracking a piece of the core and collecting the gas released from that process. in the process; An amount of methane is leaking. in addition to; The pulverized lump may not accurately represent the coal sample as a whole which may lead Thad to estimate the amount of methane resource in the reservoir.

The Triaxial 100/08 can alternatively perform both tests with a single instrument on the same sample Ag actual tank temperature and pressure conditions. in addition to; The 3-axis NMR machine can be used for:

a. Better understanding of methane flux modulation through reservoir fissures» b. understand the adsorption process at specific temperature and stress conditions;

c. Evaluation of desorption rate and production as a function of change in stresses; Dr.. a better understanding of the process of forcing water to entrap pores once the methane is released; H. Study the effect of water injection on adsorption and methane production; And the. Matrix Comparative Evaluation of Crack Permeability as a Function of Pressure and Temperature; ‎OBY 5 g. Use the pore pressure injection method to create a crack and assess the placement of the abutment; crack closure; fracturing fluid dispersion; prop flow back; failure or cracking of the stent; the ability to preserve fraction as a function of pressure and flow; And the supportive inclusion with the composition » h. use of an independent axial pressure piston to create a mechanical crack and study the fluid flow; i. use of an independent coaxial alga piston to pulverize the entire sample and collect residual gas information; or 10 j. To use intact pulp or pulverized lll to study the methane adsorption process to study the maximum total tank capacity to understand methane maturity or migration. In an alternate example of AT for operation; The sample can be cement or drilling fluid used to develop hydrocrion and tested under borehole bottom pressure and temperature conditions. The three-axis NMR device can be used to test the sample at bottomless pressure and temperature conditions for: a1. Determining the test time of cement thickness under three-gall downhole conditions b. Determine the cement preparation and curing time and record the dynamic changes before; during and after processing and preparation; c. free water measurement before and after cement setting to assess cement hydration and sealing ability; Dr.. inject the fluid into the sample to assess the permeability of the cement matrix; H. Measurement of sealing strength and effectiveness between granules, reservoir rock and coating materials; And the. measure the dispersion of solid additives; or liquid; or gaseous during cement installation and curing;

g. perform a hydrostatic compressive strength test on the specified cement and determine the leakage and sealing capacity during the various stages prior to failure (daa Jad); h. Carry out a triaxial compressive strength test on the selected cement and determine the sealing and sealing capacity during a different stage before Jad) and after failure; i. determination of the toxicity ratio and Young's modulus of static and dynamic cements; j. Determination of the effect of drilling fluid on the bonding capacity of cement with reservoir and liner rocks; K. Determination of the effect of the acidizing and fracturing fluid on cement; to. The study of the migration of gases m. Measurement of electrical properties and acoustic velocity to calibrate 0 cad ill records. Determine the effect on drilling fluid properties as a function of temperature and pressure changes. Determine the effect on the rheology of drilling fluids as a function of circulation rate and temperature or pressure between the pump and the bit. Evaluation of salt crystallization and precipitation solids; s. Evaluation of the bridging capacity of all fluid 15 riyals. Determination of the thickness of the slurry layer with the circulation of a fluid All Sh. Evaluation of filter generation and penetration into the reservoir» and T. To determine the effect on the ability of the drilling fluid to hold the drilling bits. On some ez Sail) the current detection provides the intensity; 5 (NMR, resistivity; and acoustic measurements of fluids presented and produced as a single-phase fluid at tank conditions. For example, in some cases, 0 a fluid consists of a hydrocarbon liquid and gases at a given pressure and temperature. A decrease in temperature or pressure can cause Converting a single-phase fluid into gas and liquid phases.

— 2 2 — therefore; Testing samples at reservoir conditions allows for a more accurate assessment of mixed gas-liquid samples as they exist at reservoir conditions. in other models; The present disclosure also provides “resistance NMR; acoustic and volume measurements of each separate phase “cu” brine”; “le” factor (EOR) at a chosen temperature and pressure. In cial models the present disclosure provides a measurement of sample deformation as a function of stress.

Another use of the triaxial NMR instrument is to combine NMR test and measurement data with acoustic resistivity, resistivity (induction logs), gamma, porosity (neutron logs), and geochemical logs. The data can then be extrapolated into HY) as the samples have not yet been analyzed. The use of AT with a triaxial NMR device related to fluid analysis is the accurate determination of pressure

0 saturation (bubble point) During CCE an additional feature can be 'phase identification' if more than one phase is present; Combined with NMR, acoustic measurements, and electrometry at the same time. The advantage of performing a CCE test using a triaxial NMR device compared to existing methods is that it can provide time-dependent separation and separation of different fluids based on their densities. This data can help produce the reservoir near

5 of saturation pressure and for analysis of condensate tanks. Although the forms of this disclosure are described in detail; it must be understood that it is possible to implement changes; substitutions; And modifications here without deviating from the fase and the scope of disclosure. Consequently; The scope of disclosure shall be determined by the following protections and their appropriate legal rewards. The singular accusative and accusative forms refer to the plural forms; If not stated otherwise

Clearly. Optional or GA means that the event or condition described later may or may not occur. The description includes cases in which the event or condition occurs and others in which it does not. Ranges can be expressed here starting with a single dad sodas approximate to another specific value approx. When Jie is expressed for this range it must be understood that the other form is of the same value

— 3 2 — set to the other specified value; Along with all blends within the mentioned range. in addition to; Ranges should be understood to include all values that are understood by those skilled in the field that fall within the detection range; including all values considered equivalents; They are the same or close to the specific values described. as used here dg appended claims; The words 'contain' are intended to contain 'contain'. and 'includes' and all grammatical alternatives to having an open, unrestricted meaning that does not exclude additional elements or steps.

Claims (1)

protection elements 1- A three-axis nuclear magnetic resonance device for testing the properties of a liad sample, including a device Triaxial NMR: Three axle bearing frame encapsulates: A three-axis load cell has a three-axis sample stand and defines a radial space surrounding the stand triaxial sampler; piston assembly having a piston member; To engage a structural member of a three-axle load frame » and chamber piston ; At least one end cap is able to actuate to contact the three-axle load cell where it engages The piston chamber has at least one end cap; so that the end cap is pushed axially apart from the piston chamber 0; When an axial pressure fluid is supplied to the piston chamber; to apply axial pressure on test sample; NMR instrument; An axial pressure line is in fluid contact with the piston chamber of the piston assembly; and line a bound pressure in contact by means of a fluid with the radial space; and a pore pressure line in contact 5 via a fluid with the test sample; be the axial pressure line; restricted pressure line; and line Porous pressure are independent and separate fluid flow paths. 2. Device By of claim 1; Where the constraining pressure line and the pore pressure line run across At least one end cap. 3. Device Gy of claim 1 or 2; Where at least one end cap includes: Interoperable conductor for electric current flow. 4- Device Gy of claim 1; Where at least one end cap also defines one or more 5-cavities to house at least one acoustic sensor. 5 - the device according to claim 1; Where the device is operable to maintain an axial pressure greater than constrictive pressure and greater than pore pressure. 6- Device By of claim 1; Where the test sample is cement. 7. The device according to claim 1; Where the test sample is a drill bit. 8- Apparatus according to claim 1 wherein the test sample is coal bed methane tank core. 9. A method of using the triaxial NMR apparatus mentioned in claim 1. The method includes: obtaining the test sample; load the test sample into the 3-axle sample test stand; 5 Load the three-axle sample holder into a three-axle load cell to create a loaded three-axis load cell; applying axial pressure by providing an axial pressure fluid through an axial pressure line into the piston chamber such that the end cap is pushed axially away from the piston chamber and the end cap applies axial pressure on the sample; 0 Apply a restricting pressure by supplying the constraining pressure fluid through the constraining pressure line; The bound pressure is less than and independent of the axial pressure; Circulate the temperature control fluid around the triaxial sample holder by supplying the temperature control fluid through the temperature control flow line; f Measurement data from a nuclear magnetic resonance machine. — 6 2 — 0 - Method Gy of claim 9) also includes the application of pore pressure by supplying the pore pressure fluid through the pore pressure line, where the pore pressure is less than and independent of the axial pressure and the constraining pressure. 11- Method Gy of claim 10) where the axial pressure is in the axial pressure range from 9 kPa to 3,450,000 kPa; where the bound pressure is in the restricted pressure range from 6.89 kPa to 214,000 kPa; and where the pore pressure is In the pore pressure range between 6.89 kPa to 207,000 kPa. 0 12- Method in accordance with any Claims 9-11; The method also includes measuring data from at least one acoustic sensor and at least one electrical sensor. 3- Method (Gg) of claim 9) where the test sample (Ble) is for wellbore cement. The method also includes conducting tests on wellbore cement. 4. The method in accordance with claim 9; Where the test due is drill bits and method Wa includes tests on drill bits. 5- The method according to claim 9 where the test is due Ble on core from a coal bed methane tank 0 and the Waal method includes conducting tests on the core from a coal bed methane tank. am jah and A Loy he Farid i i i X > A { except > % % I : . : q a vis Fo ¥ ie Te i ET > 1 ah no” > 3 o i a Sa x Ta BR 5 HT wer” rs i J ss i LT ded jah sabe YAMA JAM TANUD MM Sn DAH NAH AAM AJ NESS - TRE ass tase Ahaa Amit Hafa Aat L A N A Spo FS] 7 SR qo i (el Th 8 Hy 3 > AB oF ii i A HEY Ea FAR es Pwaj A Nickel LL Eva. 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