# US 9,518,904 B2 · System and method of quantifying impurities mixed within a sample of hydrogen gas

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- Number: US 9,518,904 B2
- Document ID: US9518904B2
- Status: Granted
- Kind: B2
- Application number: 14/320,729
- Filed: 2014-07-01
- Published: 2014-10-23
- Granted: 2016-12-13
- Earliest claimed: 2011-12-07
- Applicants: Peter R. Bossard; Luis Breziner; Paolo Moreschini
- Inventors: Peter R. Bossard; Luis Breziner; Paolo Moreschini
- Web page: https://patentgrep.com/patent/US9518904B2

## CPC

- G01N 7/10: by allowing diffusion of components through a porous wall and measuring a pressure or volume difference
- C01B 3/501: by diffusion
- G01N 1/4005: {by transferring a selected component through a membrane}
- G01N 33/005: {H2}
- 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)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

A system and method of taking a sample of hydrogen gas and reducing the hydrogen concentration by a factor greater than 1×108 while increasing the partial pressure of the contaminating gases by a factor greater than 100, so that extremely low levels of contamination can be accurately detected. A sample of hydrogen gas is captured. Only the hydrogen gas is removed leaving all the contaminating gases in the collection chamber. This causes the total pressure of the gas sample within the collection chamber to decrease dramatically since most of the gas was hydrogen. All the contaminants remain in the collection chamber. None are lost through pumping. As such, the concentration of contaminants within the remaining sample increases dramatically. The residual partial pressures of the contaminating gases within the collection chamber and can now be measured by a variety of techniques.

## Claims

### Claim 1

A method of determining a concentration level for impurities in a gas sample that is mostly hydrogen, said method comprising the steps of:
providing a hydrogen separator wherein a collection space and a diffusion space are separated by a hydrogen permeable membrane;
filling said collection space with said gas sample, wherein said hydrogen permeates through said hydrogen permeable membrane into said diffusion space, therein providing said diffusion space with a partial pressure of hydrogen;
sweeping said diffusion space with a sweep gas, therein lowering said partial pressure of hydrogen in said diffusion space;
measuring a pressure in said collection space, wherein said pressure is indicative of said concentration level for said impurities in said gas sample; and
removing said impurities from said collection space by introducing hydrogen into said diffusion space, wherein hydrogen diffuses through said hydrogen permeable membrane into said collection space to displace said impurities.

### Claim 2 (depends on 1)

The method according to claim 1, further including a step of venting said diffusion space prior to said step of sweeping said diffusion space.

### Claim 3 (depends on 1)

The method according to claim 1, further including a step of lowering said partial pressure of hydrogen pressure in said diffusion space with a vacuum pump.

### Claim 4 (depends on 1)

The method according to claim 1, wherein said step of sweeping said diffusion space with a sweep gas includes sweeping said diffusion space with an inert gas that does not react with hydrogen.

### Claim 5 (depends on 1)

The method according to claim 1, wherein said step of sweeping said diffusion space with a sweep gas includes sweeping said diffusion space with a reactive gas that does react with hydrogen.

### Claim 6 (depends on 1)

The method according to claim 1, further including a step of identifying said impurities remaining in said collection space with a secondary instrument.

### Claim 7 (depends on 6)

The method according to claim 6, wherein said step of identifying said impurities further includes the step of venting said collection space to a larger volume to create a lower pressure for said impurities that can be utilized as a test sample by said secondary instrument.

### Claim 8 (depends on 6)

The method according to claim 6, further including steps of drawing said impurities into an injector, and injecting said impurities into said secondary instrument.

### Claim 9 (depends on 6)

The method according to claim 6, further including a step of passing said impurities through a gas chromatography column prior to introducing said impurities into said secondary instrument.

### Claim 10 (depends on 6)

The method according to claim 6, wherein said impurities are swept toward said secondary instrument with a carrier gas and said method further includes a step of using a splitter to separate most of said sweep gas from said impurities.

### Claim 11 (depends on 10)

The method according to claim 10, further including a step of drawing gases from said collection space with at least one vacuum pump.

### Claim 12

A method of determining a concentration level of impurities in a gas sample that is mostly hydrogen, said method comprising the steps of:
providing a hydrogen separator having a collection space and a diffusion space separated by a hydrogen permeable membrane;
introducing said gas sample into said collection space, wherein said hydrogen permeates through said hydrogen permeable membrane into said diffusion space, therein providing said diffusion space with a partial pressure of hydrogen and creating a first concentration of said impurities in said collection space;
sweeping said diffusion space with an inert gas, therein further dropping said partial pressure of hydrogen in said diffusion space and creating a second concentration of said impurities in said collection space;
sweeping said diffusion space with a reactive gas, therein still further lowering said partial pressure of hydrogen in said diffusion space;
measuring a pressure in said collection space, wherein said pressure is indicative of said concentration level of total impurities in said gas sample.

### Claim 13 (depends on 12)

The method according to claim 12, further including the step of identifying said impurities remaining in said collection space with a secondary instrument.

### Claim 14 (depends on 13)

The method according to claim 13, further including the steps of drawing said impurities into an injector, compressing said impurities within said injector, and injecting said impurities into said secondary instrument.

### Claim 15 (depends on 13)

The method according to claim 13, wherein said step of identifying said impurities further includes the step of venting said collection space to a second space where optical measuring techniques are utilized to quantify impurities.

### Claim 16 (depends on 12)

The method according to claim 12, further including the step of providing a contaminant specific getter and removing at least one contaminant with said getter.

### Claim 17 (depends on 16)

The method according to claim 16, wherein said step of removing said impurities includes introducing various getters into the collect space and absorbing particular contaminating gases for release at a later time.

### Claim 18 (depends on 17)

The method according to claim 17 further including the step of drawing gases from said collection space with at least one vacuum pump.
