Automatic gas sorption apparatus and method

Patent metadata

Field	Value
Publication number	US-11307129-B2
Application number	US-202016826789-A
Country	US
Kind code	B2
Filing date	Mar 23, 2020
Priority date	Mar 23, 2020
Publication date	Apr 19, 2022
Grant date	Apr 19, 2022

Abstract

Automated apparatuses for use in examining gas sorption materials are described. Devices utilize a noncontact magnetic induction heating approach for controlling the temperature of tested materials. The apparatuses can be used to generate single or multiple isotherms simultaneously. The apparatuses can examine nanogram or microgram-scale quantities of materials of interest and can do so automatically and unattended. Pressure-composition isotherms can be provided through use of disclosed apparatuses in a period of a few hours.

First claim

What is claimed is:

1. A gas sorption apparatus comprising:
a first sample holder;
a gas inlet to the first sample holder, the gas inlet comprising a first valve;
a gas outlet from the first sample holder, the gas outlet comprising a second valve;
a heating system comprising a magnetic induction heating coil, where the first sample holder is locatable within a magnetic field of the magnetic induction heating coil; and
a control system in communication with the first valve, the second valve, the first sample holder, and the magnetic induction heating coil, the control system being configured to selectively control operation of the first valve to allow a controlled amount of a gaseous sample to be fed to the first sample holder, the control system being configured to selectively control operation of the second valve to allow a controlled amount of the gaseous sample to be removed from the first sample holder, the control system being configured to selectively control current flow through the magnetic induction heating coil to control the temperature of a gas sample within the first sample holder.

2. The gas sorption apparatus of claim 1 , wherein the first sample holder defines an internal volume of from about 0.5 milliliters to about 10 milliliters.

3. The gas sorption apparatus of claim 1 , wherein the first sample holder defines a U shape.

4. The gas sorption apparatus of claim 1 , further comprising a second sample holder in communication with the control system, the second sample holder being locatable within the magnetic field of the magnetic induction heating coil simultaneously with the first sample holder.

5. The gas sorption apparatus of claim 1 , further comprising a temperature sensor associated with the first sample holder, the control system being configured to selectively control current flow through the magnetic induction heating coil based on measurement signals received from the temperature sensor to adjust the temperature of a gas sample within the first sample holder.

6. The gas sorption apparatus of claim 1 , further comprising a pressure sensor associated with the first sample holder, the control system being configured to selectively control operation of the first and second valves based on measurement signals received from the pressure sensor.

7. The gas sorption apparatus of claim 1 , further comprising a temperature sensor and a pressure sensor, the control system being configured to collect data continuously or periodically from the temperature sensor and the pressure sensor.

8. The gas sorption apparatus of claim 7 , the control system being configured to analyze the collected data and provide a pressure-composition isotherm diagram.

9. The gas sorption apparatus of claim 1 , the control system being configured to modify the controlled operation of the first and/or second valve and thereby modify the controlled amount of a gaseous sample to be fed to or removed from the first sample holder.

10. A method for examining sorption characteristics of a gaseous sample comprising:
introducing or removing a first aliquot of a gaseous sample to/from a sample holder, the sample holder comprising a sorption material and a magnetic material;
controlling the temperature of the gaseous sample and the sorption material within the sample holder by controlled use of a magnetic induction heating coil, wherein the magnetic material is within a magnetic field of the magnetic induction heating coil and wherein the magnetic material is in thermal communication with the sorption material;
measuring a change in pressure within the sample holder following the introduction or removal of the first aliquot of the gaseous sample to/from the sample holder to determine a first equilibrium pressure of the gaseous sample with the sorption material;
automatically repeating the introducing, controlling, and equilibrium pressure determination steps a plurality of times; and
developing a first pressure-composition isotherm diagram from data collected during the repetitions.

11. The method of claim 10 , wherein the step of introducing or removing the first aliquot of the gaseous sample to/from the sample holder comprises measuring a second change in pressure within the sample holder during the introduction or removal of the first aliquot.

12. The method of claim 11 , wherein the second change in pressure is from about 5 Torr to about 50 Torr.

13. The method of claim 11 , the method further comprising modifying the second change in pressure over the course of repeating the introducing, controlling, and equilibrium pressure determination steps a plurality of times.

14. The method of claim 10 , wherein the magnetic material is in the form of particles.

15. The method of claim 10 , wherein the particles comprise composite particles including the magnetic material and the sorption material.

16. The method of claim 10 , wherein the sorption material comprises a hydrogen sorption material.

17. The method of claim 16 , the hydrogen sorption material forming a metal hydride upon interaction of the sorption material with hydrogen.

18. The method of claim 16 , wherein the sorption material preferentially adsorbs and/or desorbs a first hydrogen isotope over a second hydrogen isotope at a temperature and a pressure.

19. The method 10 , further comprising:
introducing or removing a second aliquot of a second gaseous sample to/from a second sample holder, the second sample holder comprising a second sorption material and a second magnetic material;
controlling the temperature of the second gaseous sample and the second sorption material within the second sample holder by controlled use of the magnetic induction heating coil, wherein the second magnetic material is within the magnetic field of the magnetic induction heating coil and wherein the second magnetic material is in thermal communication with the second sorption material;
measuring a change in pressure within the second sample holder following the introduction or removal of the second aliquot of the second gaseous sample to/from the second sample holder to determine a second equilibrium pressure of the second gaseous sample with the second sorption material;
automatically repeating the introducing, controlling, and equilibrium pressure determination steps involving the second sample holder a plurality of times; and
developing a second pressure-composition isotherm diagram from data collected during the repetitions; wherein
the first pressure-composition isotherm diagram and the second pressure-composition isotherm diagram are developed simultaneously.

20. The method of claim 10 , wherein the repetition is continued until a pressure within the sample holder reaches about 2000 Torr.

Assignees

• Savannah River Nuclear Solutions Llc

Inventors

• Hunyadi Murph Simona E
• Sessions Henry T
• Brown Michael A

Classifications

• G01N7/02 Primary

  by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder {(absorption bulbs B01D53/00)} · CPC title

• G01N15/0806 Primary

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

• G01N2015/0866

  Sorption · CPC title