Automated apparatus for characterization of fluid-solid systems

Patent metadata

Field	Value
Publication number	US-12352773-B2
Application number	US-202418647985-A
Country	US
Kind code	B2
Filing date	Apr 26, 2024
Priority date	May 10, 2021
Publication date	Jul 8, 2025
Grant date	Jul 8, 2025

Abstract

Embodiments of the present disclosure generally relate to apparatus, systems, and methods for characterizing fluid-solid systems. In an embodiment, a method includes placing a porous rock sample in a core holder, contacting the porous rock sample with a fluid to create a fluid-solid system inside the core holder, automatically adjusting a temperature and/or pressure of the fluid-solid system to a preselected value via a processor and at least one automated valve, monitoring the fluid-solid system for equilibrium, recording a value for temperature, pressure, and/or mass of the fluid-solid system, performing an action based on the recorded data, and repeating the adjusting, monitoring, recording, and performing operations to produce a thermodynamic data characteristic of the fluid-solid system. In one example, the performing operation includes analyzing a pressure signal for stationarity by performing an Augmented Dickey-Fuller (ADF) test and/or a Kwiatkowski-Phillips-Schmidt-Shin (KPSS) test.

First claim

What is claimed is:

1. An apparatus for characterizing a fluid-solid system, the apparatus comprising:
an environmental chamber;
a core holder disposed inside the environmental chamber;
a pressure sensor configured to sense a pressure within the core holder and produce a pressure signal;
a mass comparator operationally connected to the core holder; and
a pressure and flow control system comprising:
a pressure source in selective fluid communication with the core holder;
an automated pressure valve configured to control pressure within the core holder; and
a processor configured to:
control the automated pressure valve based at least in part on the pressure signal; and
step the pressure within the core holder through a series of predetermined pressure set points.

2. The apparatus of claim 1 , wherein the processor is further configured to:
control the pressure within the core holder to a first predetermined pressure set point;
analyze the pressure signal for stationarity; and
open the automated pressure valve for a calculated period of time to control the pressure within the core holder to a second predetermined pressure set point.

3. The apparatus of claim 2 , wherein the processor is further configured to analyze the pressure signal for stationarity by an Augmented Dickey-Fuller (ADF) test, a Kwiatkowski-Phillips-Schmidt-Shin (KPSS) test, or both.

4. The apparatus of claim 2 , wherein the processor is further configured to calculate the calculated period of time by:
performing a series of short valve openings in order to generate a series of data; and
analyzing the series of data in order to calculate the calculated period of time.

5. The apparatus of claim 1 , further comprising:
a vacuum source in selective fluid communication with the core holder; and
an automated vacuum valve configured to control pressure within the core holder, wherein the processor is further configured to control the automated vacuum valve.

6. The apparatus of claim 1 , wherein:
the environmental chamber comprises a temperature sensor;
the environmental chamber comprises a heating element, a cooling element, or combinations thereof; and
the processor is further configured to control a temperature within the environmental chamber.

7. The apparatus of claim 1 , further comprising:
an atmospheric purge mechanism configured to purge an interior of the environmental chamber of oxygen;
a source of non-reactive gas in selective fluid communication with the interior of the environmental chamber; and
an automated purge valve configured to control a flow of the non-reactive gas into the environmental chamber, wherein the processor is further configured to control an atmosphere within the environmental chamber via the automated purge valve.

8. The apparatus of claim 1 , further comprising a gas chromatograph operably connected to the core holder, wherein the processor is further configured to automatically direct contents of the core holder into the gas chromatograph.

9. The apparatus of claim 1 , wherein:
the processor is further configured to automatically log data from the pressure sensor and the mass comparator;
the core holder is a first core holder, the apparatus comprising at least a second core holder disposed inside the environmental chamber; or
combinations thereof.

10. A method of characterizing a fluid-solid system, the method comprising:
(a) placing a porous material in a core holder;
(b) contacting the porous material with a fluid to create a fluid-solid system inside the core holder;
(c) automatically adjusting a temperature of the fluid-solid system, a pressure of the fluid-solid system, or both, to a preselected value via a processor and at least one automated valve, the at least one automated valve is a pressure control valve;
(d) monitoring the fluid-solid system for equilibrium via a pressure sensor;
(e) recording a value for temperature, a value for pressure, a value for mass, or a combination thereof, of the fluid-solid system, to provide recorded data;
(f) performing an action based on the recorded data, the performing the action comprising at least:
opening the pressure control valve for a calculated period of time;
performing a series of short valve openings in order to generate a series of data; and
analyzing the series of data in order to calculate the calculated period of time and

(g) repeating operations (c) through (f) to produce a thermodynamic data characteristic of the fluid-solid system.

11. The method of claim 10 , wherein the performing the action of operation (f) further comprises analyzing a pressure signal for stationarity, wherein the pressure signal corresponds to the pressure within the core holder, and wherein the analyzing the pressure signal for stationarity comprises performing an Augmented Dickey-Fuller (ADF) test, a Kwiatkowski-Phillips-Schmidt-Shin (KPSS) test, or both.

12. The method of claim 10 , wherein the performing the action of operation (f) further comprises:
adjusting the pressure of the fluid-solid system.

13. The method of claim 10 , wherein the performing the action of operation (f) further comprises:
calculating an average of pressure values, an average of mass values, or both, over a pre-determined time duration.

14. The method of claim 13 , wherein the adjusting the pressure of the fluid-solid system comprises introducing additional fluid into the core holder.

15. The method of claim 14 , wherein the introducing the additional fluid into the core holder comprises:
opening an automated valve for a predetermined duration of time, via the processor, the automated valve being in fluid communication with a source of pressure.

16. The method of claim 15 , wherein the source of pressure comprises a vessel of fluid, gas, or combinations thereof.

17. The method of claim 13 , wherein:
the adjusting the pressure of the fluid-solid system comprises removing at least some fluid from the core holder; and
the removing at least some fluid from the core holder comprises opening an automated valve for a predetermined duration of time, via the processor, wherein the automated valve is in fluid communication with a source of vacuum.

18. The method of claim 10 , wherein:
the core holder is disposed inside an environmental chamber; and
the method further comprises:
controlling an atmosphere within the environmental chamber via an automated purge valve, the automated purge valve being in selective fluid communication with a source of non-reactive gas;
automatically interpreting, transforming, and recording unprocessed signals from a pressure sensor, a temperature sensor, and a mass comparator into a thermodynamic data characteristic of the fluid-solid system; or combinations thereof.

Assignees

• Univ Wyoming

Inventors

• Alloush Rami
• Piri Mohammad
• Lowry Ewan W

Classifications

• G01N1/44

  Sample treatment involving radiation, e.g. heat · CPC title

• G01N33/24

  Earth materials (G01N33/42 takes precedence) · CPC title

• G01N30/06

  Preparation · CPC title

• G01N15/0806

  Details, e.g. sample holders, mounting samples for testing · CPC title

• G01N15/082

  Investigating permeability by forcing a fluid through a sample · CPC title