DoE Cleanser Screening Tests First Cleanser using Triethanolamine Preliminary W. Collins C2E2 2014 September 23.

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DoE Cleanser Screening Tests First Cleanser using Triethanolamine Preliminary W. Collins C2E September 23

Objective The objective of this screening test is to conduct a compatibility test between this compound and PEM fuel cells. The testing is done in support of a supplement to a US DoE EERE contact, DE-EE The results indicate some interaction between the compound and PEM fuel cells at the concentration and flow tested.

Test parameters Cell Size25 cm 2 ElectrodeGore-50 Loadings0.4/0.4 mgPt/cm 2 Operation Current Density1000 mA/cm 2 Cell Temperature80 0 C Inlet dew points Anode48 0 C Cathode87 0 C Exit PressuresAmbient/Ambient

Test parameters (cont) Conditions Flows Anode1.75 lpm (10) Cathode 1.55 lpm (4) Atomizer130e-06 lpm (~200 ppm) Operating Point Intentionally close to flooding (worst case) Program Break in 16 hr mV Diagnostics 5 hrs Baseline 45 hr mA/cm2 Diagnostics 1 hr Contamination 6 hrs Diagnostics 1 hr Clean up 24 hrs Diagnostics 5 hr Total103 hrs

Compound Concentration 5% of full strength (estimate after two rinses) CompositionMSDS IngredientCAS NumberPercent Range Water ≥ 78% Triethanolamine ≤ 10% Ethoxylated Alcohol ≤ 5% Propylene Glycol Butyl Ether ≤ 5% Tetrapotassium Pyrophosphate ≤ 1% Potassium Silicate ≤ 1% ColorantProprietary≤ 1%

Results Summary of Testing Break in and initial diagnostics normal Baseline normal Diagnostics after baseline normal Steady rapid decay during contamination ~22 mV/hr Diagnostics after contamination abnormal Limited recovery ~119 mV, asymptote at ~500 mV Diagnostics after clean up show limited improvement

Results (cont) Test Results: Figure 1 shows the performance history. Figure 2 shows no change in IR until attempting clean up. Figure 3A (anode) and Figure 3C (cathode) show no decay due to crossover. Figure 4A (anode) and Figure 4C (cathode) show no catalyst issues However, the Electrochemical impedance spectroscopy (EIS) shown in Figure 5 is very interesting

Results (cont) Figure 1 – Performance History Rapid decay starts upon exposure. Linear decrease during exposure. Partial clean up on DI water until asymptotes

Results (cont) Figure 2 – IR History Initial step change due to intentional ‘flooding’. Linear increase during exposure. Partial clean up on DI water until asymptotes

Results (cont) Figure 3 – X/O History Beginning of Test and End of Test data basically the same.

Results (cont) Figure 4 – Cyclic Voltammetry History Beginning of Test and End of Test data basically the same.

Results (cont) Figure 5 – Electrochemical impedance spectroscopy (EIS)

Results (cont) Test Results (cont): The difference between the measurements at the beginning of the test and beginning of contamination are slight and may be due to saturation of the cathode GDL. The difference between the measurements at the beginning of contamination and end of contamination are notable. Frequency magnitude from right to left. Right is 0.1 Hz and represents issues in mass transport issues Left is 10 kHz and represents ionic and ohmic resistance Looks to be mass transport issues. The difference between the measurements at the end of contamination and end of test are also notable. They mirror the recovery.

What does this mean? Assumptions: Ingest 14 cc’s of 100% cleanser during a 7 kg fill Operate at ~1/4 power (1000 mA/cm2) for 14 hrs (est. range on 7 kg) Results: Operating at extreme conditions Assumptions may be too conservative Decay is 0.2 mA/cm2 prior to contamination Decay is ~22 mA/cm2 duringto contamination Clean up consisted of injecting DI water. There was a partial recovery. The EIS also improved. This may indicates mass transport issues.