# US 2013/0153441 A1 · Method and apparatus for evaluating ex-situ chemical degradation of membranes

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- Number: US 2013/0153441 A1
- Document ID: US20130153441A1
- Status: Published application
- Kind: A1
- Application number: 13/327,051
- Filed: 2011-12-15
- Published: 2013-06-20
- Earliest claimed: 2011-12-15
- Assignees: Nissan North America, Inc.
- Inventors: RAMESHWAR YADAV; KEVORK ADJEMIAN
- Web page: https://patentgrep.com/patent/US20130153441A1

## CPC

- H01M 8/1039: halogenated, e.g. sulfonated polyvinylidene fluorides
- H01M 8/008: Disposal or recycling of fuel cells
- H01M 2008/1095: {Fuel cells with polymeric electrolytes}
- Y02E 60/50: Fuel cells
- Y02W 30/84: Recycling of batteries or fuel cells
- Y10T 436/193333: In aqueous solution
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02W: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

Disclosed herein are methods and devices for evaluating ex-situ chemical degradation of fuel cell membranes. One embodiment of a method for evaluating ex-situ chemical degradation of a membrane comprises submerging a membrane in Fenton solution in a reaction vessel with a non-reactive weight configured to maximize exposure of the membrane to the Fenton solution, sealing the reaction vessel, heating the reaction vessel at a fixed rate to a predetermined temperature, holding the reaction vessel at the predetermined temperature for a predetermined test period, cooling the reaction vessel to room temperature, removing the membrane and analyzing the Fenton solution for fluoride ions.

## Claims

### Claim 1

A method for evaluating ex-situ chemical degradation of a membrane comprising the steps of:
submerging a membrane in Fenton solution in a reaction vessel with a non-reactive weight configured to maximize exposure of the membrane to the Fenton solution;
sealing the reaction vessel;
heating the Fenton solution in the reaction vessel at a fixed rate to a predetermined temperature;
holding the Fenton solution in the reaction vessel at the predetermined temperature for a predetermined test period;
cooling the Fenton solution in the reaction vessel to room temperature; and
analyzing the Fenton solution for fluoride ions.

### Claim 2 (depends on 1)

The method of claim 1, further comprising removing the membrane and the non-reactive weight from the Fenton solution prior to analyzing.

### Claim 3 (depends on 1)

The method of claim 1, wherein the non-reactive weight comprises two magnets coated in a non-reactive coating placed on opposing sides of the membrane.

### Claim 4 (depends on 1)

The method of claim 1, wherein the reaction vessel has a single sealable opening providing access to a cavity of the reaction vessel.

### Claim 5 (depends on 1)

The method of claim 1, wherein heating the reaction vessel at a fixed rate is performed in an oven.

### Claim 6 (depends on 5)

The method of claim 5, wherein holding the predetermined temperature is performed in the oven.

### Claim 7 (depends on 1)

The method of claim 1, wherein the predetermined temperature is 80° C. or greater.

### Claim 8 (depends on 1)

The method of claim 1, wherein analyzing the Fenton solution is performed with a meter having an ion selective electrode.

### Claim 9 (depends on 1)

The method of claim 1, wherein the steps are performed on a plurality of membranes, each membrane submerged in Fenton solution in a respective reaction vessel with a respective non-reactive weight.

### Claim 10 (depends on 9)

The method of claim 9, wherein each of the plurality of membranes are identical and the predetermined test period is different for each of the plurality of membranes.

### Claim 11 (depends on 9)

The method of claim 9, wherein the plurality of membranes are each different and the predetermined test period is the same for each of the plurality of membranes.

### Claim 12

A test assembly for measuring the chemical degradation of a membrane comprising:
a reaction vessel having a single sealable opening;
Fenton solution;
a non-reactive weight configured to retain the membrane submerged in the Fenton solution while providing maximum exposure of the membrane to the Fenton solution;
means for heating the reaction vessel at a fixed rate;
means for maintaining the reaction vessel at a fixed temperature; and
means for analyzing fluoride ions in the Fenton solution.

### Claim 13 (depends on 12)

The test assembly of claim 12, wherein the Fenton solution is hydrogen peroxide and ferrous sulfate heptahydrate.

### Claim 14 (depends on 12)

The test assembly of claim 12, wherein the weight comprises two magnets coated in a non-reactive coating and configured for placement on opposing sides of the membrane.

### Claim 15 (depends on 12)

The test assembly of claim 12, wherein the means for analyzing is a meter having an ion selective electrode.

### Claim 16 (depends on 12)

The test assembly of claim 12 further comprising additional reaction vessels each having a single sealable opening.

### Claim 17 (depends on 12)

The test assembly of claim 12, wherein the means for heating the reaction is an oven.

### Claim 18 (depends on 12)

The test assembly of claim 12, wherein the means for maintaining is an oven.

### Claim 19 (depends on 18)

The test assembly of claim 18, wherein the means for heating the reaction is the oven.

### Claim 20

A test assembly for simulating chemical degradation of a polymer electrolyte membrane comprising:
a reaction vessel having a single sealable opening;
a solution of hydrogen peroxide and ferrous ions;
two micro-magnetic bars having a non-reactive coating, the bars configured to retain the membrane submerged in the Fenton solution while providing maximum exposure of the membrane to the Fenton solution;
an oven; and
a meter for analyzing fluoride ions in the solution.