NASA Technical Reports Server (NTRS) 20140002804: Advanced Water Purification System for In Situ Resource Utilization

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Advanced Water Purification System for 
In Situ Resource Utilization 



3 

, - c J| 



4 


Steve Anthony 

NASA Kennedy Space Center 
September 12, 2013 




In Situ Resource Utilization 



One of NASA's goals is to enable long- 
term human presence in space, 
without the need for continuous 
replenishment of consumables from 
Earth. 

In situ resource utilization (ISRU) is 
the use of extraterrestrial resources 
to support activities such as human 
life-support, material fabrication and 
repair, and radiation shielding. 

Potential sources of ISRU 
resources include lunar and Martian 
regolith, and Martian atmosphere. 



CROPS Mars ISRU Demonstration Unit 




Water and Oxygen Production from Lunar Regolith 



Water and byproducts (including 
hydrochloric and hydrofluoric acids) can 
be produced from lunar regolith via a 
high-temperature hydrogen reduction 
reaction and passing the produced gas 
through a condenser. 

900°C 

FeO + H 2 -> Fe + H 2 0 

Due to the high solubility of HCI and HF 
in water, these byproducts are expected 
to be present in the product stream (up 
to 20,000 ppm) and must be removed 
(less than 10 ppm) prior to water 
consumption or electrolysis. 



3 



Contaminant Removal Techniques 

'V'' 

• Due to their consumable nature, typical water purification methods may not be 
suitable for HCI and HF removal in extraterrestrial applications. 

• Membranes and adsorbents are often regenerated with large amounts of water 
and/or basic solutions, which aren't available in the lunar environment. 

• Naturally-occurring adsorbents may be replaced rather than regenerated. 


Method 

Examples 

Membrane 
(solute retention) 

Reverse osmosis 

Nanofiltration 

Proton Exchange 

Membrane 
(solute transport) 

Dialysis 

Electrodialysis 

Anion Exchange 


Alumina-based adsorbents 

Adsorption 

Natural adsorbents (mud, ore, 
clay, soil, chitosan) 




4 




Nafion® Membranes for Contaminant Removal 



Nafion®, a common fuel cell proton 
exchange membrane, was investigated for 
its chloride and fluoride rejection capability 
in a previous study 

The ability to reject 98-99.9% of chloride 
and 50-80% of fluoride was demonstrated 

This rate of rejection was not sufficient to 
produce electrolysis-grade water 

Since water had to diffuse across the 
membrane and be recovered in the vapor 
phase, relatively small amounts of water 
were recovered using large amounts of 
carrier gas 

Other technologies were researched with 
an emphasis on maximizing water recovery 
and contaminant removal: 

- Higher contaminant removal/rejection rate 

- Contaminant removal/water retention instead of 
contaminant rejection/water transport 

- Liquid phase only process 




b) Solution Temperature, °C 

Anthony, S.M., et al. "Contaminant Removal from Oxygen 
Production Systems for In Situ Resource Utilization." AIAA 
SPACE 2012 Conference & Exposition, AIAA 2012-5167. 


5 


Cathode 



Electrodialysis for Contaminant Removal 



Anode 












Experimental Apparatus 












Electrolyte Pump 


|Feed and Waste] 
Peristaltic Pumps 


Waste Solution 


Electrolyte 


Membrane Stack 


Feed Solution 


High Efficiency Electrodialysis (HEED®) membrane stack purchased from EET Corp. 
Stack contains 20 alternating Ralex® anion and cation exchange membranes 
0.5% NaS0 4 solution circulated through outer cells to protect electrodes 


7 




Baseline Contaminant Removal: 
20,000 ppm HCI/HF Solution 




• Starting volume 

- 500 mL diluent 

- 500 mL concentrate 

• Final volume 

- 295 mL diluent 

- 685 mL concentrate 

• Power supply 

- 30 V maximum 

- 3 A maximum 

• Pump speed 

- 100% diluent 

- 100% concentrate 

• Reached steady state 

within 30 min 



Diluent Stream 

Fluoride 

Chloride 

Initial (ppm) 

18,800 

26,400 

Final (ppm) 

71.1 

11.4 

Removal (%) 

99.44 

99.94 


8 


Power [W] 




Baseline Contaminant Removal: 
200 ppm HCI/HF Solution 



• Starting volume 

- 500 mL diluent 

- 500 mL concentrate 

• Final volume 

- 500 mL diluent 

- 500 mL concentrate 

• Power supply 

- 30 V maximum 

- 3 A maximum 

• Pump speed 

- 100% diluent 

- 100% concentrate 

• Reached steady state 

in less than 10 min 



Diluent Stream 

Fluoride 

Chloride 

Initial (ppm) 

166 

179 

Final (ppm) 

0.26 

0.07 

Removal (%) 

99.85 

99.96 


9 


Power [W] 




Variable Matrix Testing: 
Concentrate Volume 



Initial Concentrate 
Volume (mL) 

Final Diluent 
Volume (mL) 

Final Concentrate 
Volume (mL) 

Final Fluoride 
Concentration 
(ppm) 

Final Chloride 
Concentration 
(ppm) 

0 

170 

290 

550 

23 

130 

305 

310 

290 

25 

250 

335 

400 

167 

22 

500 

295 

685 

71 

11 


• Parameters: 

- Initial diluent volume: 500 mL 

- Initial diluent concentration: 20,000 ppm HCI/HF 

- Pump speed: 100% of maximum 

- Voltage: 30 V maximum 

- Current: 3 A maximum 

• 130 mL is minimum volume required to fill the concentrate membrane cells and tubing 

• Final fluoride concentration decreases substantially with decreasing initial concentrate 
volume 

• Final chloride concentration does not decrease with increasing initial concentrate 
volume below 250 mL 


10 



Variable Matrix Testing: 
Pump Speed 



Pump Speed (% of 
maximum) 

Final Diluent 
Volume (mL) 

Final Concentrate 
Volume (mL) 

Final Fluoride 
Concentration 
(ppm) 

Final Chloride 
Concentration 
(ppm) 

< 10 

500 

510 

14,500 

13,700 

20 

280 

650 

71 

8.6 

50 

300 

700 

158 

20 

100 

295 

685 

71 

11 


• Parameters: 

- Initial diluent volume: 500 mL 

- Initial diluent concentration: 20,000 ppm HCI/HF 

- Initial concentrate volume: 500 ml 

- Voltage: 30 V maximum 

- Current: 3 A maximum 

• Pump speed does not affect final fluoride and chloride concentrations, or final diluent 
and concentrate volumes at or above 20% of maximum setting (at least 200 mL/min) 

• Minimum pump speed does not appear to allow for any ion exchange 


li 



Variable Matrix Testing: 
Power Supply 



Maximum 
Voltage (V) 

Maximum 
Current (A) 

Final Diluent 
Volume (mL) 

Final 

Concentrate 
Volume (mL) 

Final Fluoride 
Concentration 
(ppm) 

Final Chloride 
Concentration 
(ppm) 

30 

3.0 

296 

685 

71 

11 

15 

3.0 

325 

675 

1,170 

47 

60 

350 

640 

26 

2.8 

30 

1.5 

355 

610 

132 

26 

6.0 

365 

685 

79 

9.8 


• Parameters: 

- Initial diluent volume: 500 mL 

- Initial diluent concentration: 20,000 ppm HCI/HF 

- Initial concentrate volume: 500 mL 

- Pump speed: 100% of maximum 

• Decreasing voltage or current increases final diluent fluoride and chloride 
concentrations 

• Increasing voltage decreases final diluent chloride and fluoride concentrations 

• Increasing current does not affect final diluent chloride and fluoride concentrations 


12 




ISRU Scenario Testing: 
Concentrate Replenishment 



Initial volumes: 

- 500 mL diluent 

- 100 mL concentrate 
(replaced every hour, 
300 mL total) 

Power supply: 

- 30 V maximum 

- 3.0 A maximum 

Pump speed: 100% 
Final volumes: 

- 250 mL diluent 

- 600 mL concentrate 

Contaminant removal 
improved versus 
baseline, but at the 
expense of longer 
processing time 


45,000 


40,000 



• - Feed Chloride 
--O — Waste Chloride 
■ Feed Fluoride 
— □ — Waste Fluoride 
- a - Power 






\d — a — o 




-Q — 


^ A- -A -A- -a- 


80 


70 


60 


50 


40 


30 


20 


10 


0 


20 40 60 

80 100 120 

Time [min] 

140 160 180 

Diluent Stream 

Fluoride 

Chloride 

Initial (ppm) 

17,000 

17,400 

Final (ppm) 

27 

3.9 

Removal (%) 

99.92 

99.99 


13 


Power [W] 




ISRU Scenario Testing: 
Diluent Replenishment 





Initial volumes: 


- 250 mL diluent 
(replaced every hour, 
1250 mL total) 

- 250 mL concentrate 

Power supply: 

- 30 V maximum 

- 3.0 A maximum 

Pump speed: 100% 
Final volumes: 

- 360 mL diluent 

- 830 mL concentrate 

Contaminant removal 
was not significantly 
improved versus 
simply processing at a 
higher diluent to 
concentrate volume 
ratio 



14 


Power [W] 




ISRU Scenario Testing: 
Obtaining Electrolysis-Grade Water 


1000 mL 
HCI/HF 
Solution 


390 mL 
Clean Water 


500mL 

130 mL 




* 


Diluent 



Concentrate 


"A" 



"A" 


500 mL 


300 mL 


Diluent 

"B" 


300 mL 


130 mL 


330 mL 


Concentrate 

Ur\U 


'B 


130 mL 


330 mL 


Diluent 

"C" 


Concentrate 
" C" 


435 mL 565 mL 130 mL 


330 mL 


Diluent 

Concentrate 

"D" 

"D" 


415 mL 


130 mL 



Diluent "A" 

Fluoride 

Chloride 

Initial (ppm) 

14,200 

15,100 

Final (ppm) 

736 

124 

Removal (%) 

94.8 

99.2 


Diluent "B" 

Fluoride 

Chloride 

Initial (ppm) 

16,200 

19,000 

Final (ppm) 

214 

126 

Removal (%) 

98.7 

99.3 


Diluent "C" 

Fluoride 

Chloride 

Initial (ppm) 

1,140 

222 

Final (ppm) 

12.6 

10.9 

Removal (%) 

98.9 

95.1 


Diluent "D" 

Fluoride 

Chloride 

Initial (ppm) 

80.4 

41.4 

Final (ppm) 

0.41 

0.16 

Removal (%) 

99.5 

99.6 


15 












Future Work: 
System Optimization 



• Added new and additional components to increase system robustness and 
minimize processing time: 

- Larger membrane stack that contains two 20 membrane cells which can run in series or parallel 

- Higher voltage/current power supply to achieve rapid equilibrium 

- In-line conductivity meters for real-time measurement of water purity 

- Hastelloy® electrodes which offer superior protection against hydrofluoric acid versus stainless steel 


DUAL CELL 

1 1 

m 

is* 

cel) cell 
’ 1 * 2 * 

• • ♦ 

% ceH „cell„ 

1 2 t 

. . . 


1 1 

HU 

PARALLEL 

SERIES 


Other considerations for future work: 

- Different types of anion/cation exchange membranes 

- Alternate membrane stack configurations 

- Integration with additional water processing unit (e.g., Nafion®) 

- Increase system automation 


http://www.eetcorp.com/lts/flowconfig.htm 


16 




Future Work: 

Mars ISRU Water Purification 



Ion 

C (wt%) 

C th (wt%) 

Na + 

0.27 

0.10 

Mg 2+ 

0.44 

0.60 

K + 

0.28 

0.03 

Ca 2+ 

0.05 

0.04 

ci- 

0.79 

0.04 

cio 4 - 

0.72 

0.60 

HC0 3 - 

0.73 

? 

so 4 2 - 

0.78 

? 


Kounaves, S.P., et al. "Aqueous Carbonate 
Chemistry of the Martian Soil at the Phoenix 
Landing Site," 40 th Lunar and Planetary Sciences 
Conference, 2009. 



Time [min] 


• Attemped to simulate ionic contaminants in water recovered by Phoenix lander 

• In absence of specific ion standards, measured contaminant removal indirectly via 
conductivity meters in diluent and concentrate streams 

• Achieved minimum diluent conductivity after about 10 min 


17 


Power [W] 




Acknowledgements 



Collaborators 


• Dr. Scott Jolley, QinetiQ North America 

• Jim Captain, QinetiQ North America 


Funding Sources 


• KSC Center Innovation Fund 

• KSC Core Technical Capabilities Program 

• KSC Independent Research & Technology Development Program 


18 



vanced Water Purification System for 
In Situ Resource Utilization 


Steve Anthony 

NASA Kennedy Space Center 
September 12, 2013