# US 11,307,129 B2 · Automatic gas sorption apparatus and method

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- Number: US 11,307,129 B2
- Document ID: US11307129B2
- Status: Granted
- Kind: B2
- Application number: 16/826,789
- Filed: 2020-03-23
- Published: 2021-09-23
- Granted: 2022-04-19
- Earliest claimed: 2020-03-23
- Assignees: Savannah River Nuclear Solutions, LLC
- Applicants: Savannah River Nuclear Solutions, LLC
- Inventors: Simona E. Hunyadi Murph; Henry T. Sessions; Michael A. Brown
- Web page: https://patentgrep.com/patent/US11307129B2

## CPC

- G01N 7/02: by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder {(absorption bulbs B01D53/00)}
- G01N 15/0806: {Details, e.g. sample holders, mounting samples for testing}
- G01N 2015/0866: {Sorption}
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## 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.

## Claims

### Claim 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.

### Claim 2 (depends on 1)

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.

### Claim 3 (depends on 1)

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

### Claim 4 (depends on 1)

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.

### Claim 5 (depends on 1)

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.

### Claim 6 (depends on 1)

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.

### Claim 7 (depends on 1)

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.

### Claim 8 (depends on 7)

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

### Claim 9 (depends on 1)

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.

### Claim 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.

### Claim 11 (depends on 10)

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.

### Claim 12 (depends on 11)

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

### Claim 13 (depends on 11)

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.

### Claim 14 (depends on 10)

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

### Claim 15 (depends on 10)

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

### Claim 16 (depends on 10)

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

### Claim 17 (depends on 16)

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

### Claim 18 (depends on 16)

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.

### Claim 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.

### Claim 20 (depends on 10)

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