# US 10,502,673 B2 · Apparatus and methodology for measuring properties of microporous material at multiple scales

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- Number: US 10,502,673 B2
- Document ID: US10502673B2
- Status: Granted
- Kind: B2
- Application number: 15/935,151
- Filed: 2018-03-26
- Published: 2018-07-26
- Granted: 2019-12-10
- Earliest claimed: 2013-02-08
- Assignees: Schlumberger Technology Corporation
- Applicants: Schlumberger Technology Corporation
- Inventors: Maxim Andreevich Chertov; Roberto Suarez-Rivera; Dean M. Willberg; Sidney J. Green
- Web page: https://patentgrep.com/patent/US10502673B2

## CPC

- G01N 15/082: {Investigating permeability by forcing a fluid through a sample}
- G01N 7/00: Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N 15/08: Investigating permeability, pore-volume, or surface area of porous materials
- G01N 15/0806: {Details, e.g. sample holders, mounting samples for testing}
- G01N 15/0826: {and measuring fluid flow rate, i.e. permeation rate or pressure change}
- G01N 15/088: {Investigating volume, surface area, size or distribution of pores; Porosimetry}
- G01N 33/24: Earth materials (G01N33/42 takes precedence)
- 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

A method for characterizing properties of a sample that employs a test apparatus including an isolated sample cell and pressure sensor where the isolated sample cell is loaded with the sample and gaseous test fluid to perform a number of different tests to derive properties of the sample. The tests can be performed over different parameters, such as different applied pressures of the test fluid to derive parameters related to apparent gas permeability of the sample as a function of applied pressure, different gaseous test fluids to characterize dependence of permeability of the sample on mean free molecular path or pressure, with both adsorptive and non-adsorptive test gases to characterize at least one property related to adsorptive interaction between the adsorptive test gas and the sample, and with samples of varying saturation levels to derive a measure of at least one property of the subsamples at corresponding saturation levels.

## Claims

### Claim 1

A method for characterizing properties of a sample under test, comprising:
a) providing a test apparatus including a sample cell and associated pressure sensor, wherein the sample cell has a configuration where the sample cell is filled with test fluid under pressure and isolated from other parts of the test apparatus, and wherein the pressure sensor of the test apparatus has a configuration that measures pressure of the sample cell when the sample cell is isolated from other parts of the test apparatus;
b) using the test apparatus with the sample cell loaded with the sample under test and a source of a first gaseous test fluid to perform a test with the first gaseous test fluid where the pressure sensor of the test apparatus is configured to measure pressure of the sample cell over time when the sample cell is isolated from other parts of the test apparatus in order to derive a measure of permeability of the sample under test with respect to the first gaseous test fluid;
c) using the test apparatus with the sample cell loaded with the sample under test and a source of a second gaseous test fluid to perform a test with the second gaseous test fluid where the pressure sensor of the test apparatus is configured to measure pressure of the sample cell over time when the sample cell is isolated from other parts of the test apparatus in order to derive a measure of permeability of the sample under test with respect to the second gaseous test fluid; and
d) combining the permeability measurements of b) and c) for user evaluation;
wherein the first gaseous test fluid is different from and heavier than the second gaseous test fluid.

### Claim 2 (depends on 1)

A method according to claim 1, wherein the combined results of d) characterize dependence of apparent permeability of the sample under test on mean free molecular path of a gaseous fluid or pressure.

### Claim 3 (depends on 1)

A method according to claim 1, wherein the combining of d) involves translation of the permeability measurements of one of b) and c) according to a parametric equation.

### Claim 4 (depends on 3)

A method according to claim 3, wherein the parametric equation has the form
k
G
⁢
⁢
2
⁡
(
λ
G
⁢
⁢
2
λ
G
⁢
⁢
1
·
P
)
=
k
G
⁢
⁢
2
⁡
(
(
μ
M
)
G
⁢
⁢
2
/
(
μ
M
)
G
⁢
⁢
1
·
P
)
=
k
G
⁢
⁢
1
⁡
(
P
)
,
where kG1 is the permeability of the sample under test with respect to the first gaseous test fluid,
kG2 is the permeability of the sample under test with respect to the second gaseous test fluid,
λG1 is the free mean molecule path with respect to the first gaseous test fluid,
λG2 is the free mean molecule path with respect to the second gaseous test fluid,
(
μ
M
)
G
⁢
⁢
1
is the ratio of the gas viscosity μ to the square root of the molar mass M for the first gaseous test fluid,
(
μ
M
)
G
⁢
⁢
2
is the ratio of the gas viscosity μ to the square root of the molar mass M for the second gaseous test fluid, and
P is pressure.

### Claim 5 (depends on 1)

A method according to claim 1, wherein the first gaseous test fluid and the second gaseous test fluid are selected from monoatomic gases, diatomic gases, or combinations thereof.

### Claim 6 (depends on 1)

A method according to claim 1, further comprising:
performing calibration operations of the test apparatus with both the first gaseous test fluid and the second gaseous test fluid; and
using the results of the calibration operations in deriving the permeability measurements of b) and c).