AIAA 2015-4562

SPACE Conferences and Exposition

31 Aug-2 Sep 2015, Pasadena, California
AIAA SPACE 2015 Conference and Exposition

Survey of Perchlorate Extraction and Potential Uses on

Mars

Brian P. Franz1
University of Southern California, Los Angeles, CA, 90089, USA

James K. Villarreal2
Raytheon Company, Tucson, AZ, 85756, USA

In-situ resource utilization (ISRU) is an important consideration for any manned Mars mission. This is
especially true for the manufacture of oxygen for both respiration and as an oxidizer for rocket propellant.
To this end, the literature focuses primarily on conversion of the carbon dioxide Martian atmosphere through
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various means. Proposed herein is an alternative method that makes use of the perchlorates found in the
Martian regolith. Mars offers an abundant source of this material with confirmed measured concentrations
upwards of one percent from two landing sites. A summary of methods for extracting perchlorate compounds
and separating them into more useable constituents is discussed. A number of uses for the raw materials are
discussed, including in-situ oxygen production and solid oxygen candles. An additional and promising use is
direct mixing of the perchlorate compounds as the solid oxidizer in a solid rocket motor configuration using
suitable binder and fuel combinations.

I. Background and Rationale

S pace exploration has been both a triumph and a struggle for the human race since the dream of leaving Earth
became reality over 60 years ago. In this evolution the primary restrictive factor involves the propellant,
specifically the method and efficiency in which propellant is expelled. The industry is fast-approaching the limit for
improvements in chemical propulsion specific impulse [1], measured as the efficiency in which a mass of propellant
is converted to useable thrust impulse. Space missions have turned to alternative forms of power and propulsion in
order to boost specific impulse thusly circumventing the chemical propulsion efficiency limit at the expense of
lower thruster and therefore longer flight times. In this way low-thrust, high efficiency electrical and nuclear power
propulsion systems are a necessary step in the advancement of propulsion due to their achievable efficiency [2].

In addition to advances in increasing propulsion specific impulse, a barrier every current propulsion system
must handle is the necessity to carry all of the storable propellant for the mission duration. An expectation would be
solar propulsion or beamed energy systems; both in their infancy. The ability to reduce or eliminate this barrier
would directly benefit the ability to send unmanned and manned missions further into the cosmos. In-situ resource
utilization (ISRU) of space bodies that are within reach with current propulsion technologies is a fundamental and
necessary next step in crossing this barrier and advancing space exploration.

Mars has been an emphasis for current endeavors in space exploration for reasons including the similarities to
Earth, determination of how Earth-like planets form, and search for evidence of past or existing life. From Spirit,
Opportunity and Curiosity that have roamed the surface, to Mars Reconnaissance Orbiter (MRO), Mars Odyssey and
the Mars Atmosphere and Volatile Evolution (MAVEN) in orbit, the Red Planet has been the primary focus of our
nation’s space program for much of the last twenty years [3]. With the emergence of the private space sector and
visionaries such as Elon Musk making statements that he wants to “put a man on Mars in 10-12 years” [4], research
into the potential uses of the resources on Mars will become vital to the success of future missions.

Current developments for ISRU on the surface of Mars have focused on harvesting the Martian atmosphere to
be used as a potential source of oxygen as well as liquid rocket propellant [5]. A potential alternative is to harvest
the known perchlorate content in the Martian regolith [6][7][8]. A perchlorate molecule has twice the amount of
oxygen than a carbon dioxide molecule and is a common ingredient in solid rocket propellant [9]. Couple this with

1
AIAA Student Member bfranz@usc.edu
2
AIAA Senior Member. James.K.Villarreal@raytheon.com
1
American Institute of Aeronautics and Astronautics

Copyright © 2015 by the American Institute of Aeronautics and Astronautics, Inc. All rights reserved.
 the wide-spread abundance on the Martian surface, it has the potential to be an extremely useful in-situ resource.
This alternative approach is proposed herein by an investigation into and development of a perchlorate separation
and extraction method from Martian regolith analogs. By investigating various methods of perchlorate extraction
and remediation in the terrestrial domain, a perchlorate separation and extraction system can be developed for
implementation on Mars.

II. Perchlorate Content and In-Situ Resource Extraction on Mars

Nearly every Martian lander/rover successfully sent to the Red Planet has confirmed the existence of perchlorate
(ClO4-) in the Martian regolith. From the Phoenix Lander confirmation in the northern hemisphere [7] and
Curiosity’s detection at Gale Crater’s Rocketnest [8], to the reanalysis of data from the Viking 1 and 2 landers at
mid-latitudes [6], the perchlorate content on Mars is abundant and wide-spread. The Phoenix Lander confirmed the
detection of stable magnesium perchlorate hexahydrate (Mg(ClO4)2 . 6H2O) [16]. At Gale Crater, Curiosity
confirmed the list of regolith compounds given in Table 1 and it is believed that the perchlorate compound is
calcium perchlorate (Ca(ClO4)2 . 4H2O) [10].
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Table 1: Regolith Compounds Detected by Curiosity at Gale Crater

Compound + ClO4- Chemical Formula

Pure ClO4-
Fayalite FeSiO4 + ClO4-
Hematite Fe2O3 + ClO4-
Magnetite Fe3O4 + ClO4-

In order to use the perchlorate content as a resource, the process must be understood to convert a sample of
Martian regolith to pure, useable perchlorate molecules. This process has three steps: first, the dehydration of the
regolith compounds to recover the water molecules; second, the separation of the perchlorate compound from the
regolith; and third, the separation of the perchlorate molecule from the perchlorate compound. The first step has
been experimentally verified for both the magnesium and calcium perchlorate compounds; Table 2 shows the
dehydration chemical reactions and corresponding temperatures.

Table 2: Dehydration Chemical Reactions and Corresponding Temperatures [17] [18]

Chemical Reaction Temp (̊ C)

Mg(ClO4)2 . 6H2O  Mg(ClO4)2 + 6H2O 395
Ca(ClO4)2 . 4H2O  Ca(ClO4)2 + 4H2O 329

The second step has been initially quantified for Ca(ClO4)2 by Migdal-Mikuli et al and Bruck et al. using
thermal phase change, shown in reaction (1) with the compounds listed in Table 1 to precipitate the calcium
perchlorate out of the iron ore; the results are presented in Table 3. Although only a proof of concept, this gives
credibility and validity to the pursuit of the third step as well as the process as a whole.

Ca(ClO4)2 (s)  Ca(ClO4)2 (aq) @ ≤ 400̊ C (1)

Table 3: Gale Crater Regolith Compounds and Corresponding

Ca(ClO4)2 Precipitation Temperature [10]

Compound + ClO4- Temp (̊ C) Heatflow (mW)

Pure 380 -6
Fayalite 380 -5
Hematite 375 -6
Magnetite 380 -2

The separation of the perchlorate compound into its respective molecules is an obstacle to be overcome
through chemical breakdown and recombination. A perchlorate molecule has both ionic and covalent bonds [11].
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 The bond between a calcium molecule and a perchlorate molecule is an ionic bond while the bond between the
chlorine and the oxygen molecules is a covalent bond; the order in which the molecule is broken down will
determine whether recombination is necessary as well as the energies needed in the chemical process. Bruck et al.
took the aqueous solution they developed from reaction (1) and used thermal decomposition to yield calcium
chlorite and oxygen molecules as seen in reaction (2); the temperature at which this reaction occurs is slightly
dependent upon the type of iron ore originally associated with the compound [10]. Devlin et al. quantified that the
magnesium perchlorate compound, once dehydrated, does not melt like its calcium perchlorate counterpart. Instead,
the magnesium perchlorate compound thermally decomposes first, as seen in reaction (3).

Ca(ClO4)2 (aq)  CaCl2 (s) + 4O2 (g) @ ≥ 400̊ C (2)

Mg(ClO4)2 (s)  MgO (s) + Cl2 (g) + 7/2O2 (g) @ > 470̊ C (3)

This method would require extensive chemical dissociation and recombination processes that would include
the breaking of the ionic bond between calcium and chlorine and the covalent bond between the oxygen molecules
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and then recombining the oxygen and the chlorine to produce the desired perchlorate compound as seen in reactions
(4) and (5), listed below. A list of the needed chemical reactions and associated theoretical energies is found in
Table 4 where a positive energy denotes an endothermic reaction (i.e. it takes energy to break down the compound).
An added benefit to this method is the potential to use the byproducts of water, magnesium and calcium content in
other in-situ applications.

CaCl2  Ca2+ + 2Cl- (4)

4O2 + 2Cl-  2ClO4- (5)

Table 4: List of Necessary Reactions and Bond Energies for

Chemical Dissociation and Recombination [12]

Reaction Energy (kJ/mol)

2+ 2-
MgO  Mg + O 3,795
2+ -
CaCl2  Ca + 2Cl 2,268
- -
Cl-Cl  Cl + Cl 242
2- 2-
O=O  O + O 498
- 2- -
Cl + O  ClO -272.4
- 2- -
ClO + O  ClO2 -243.1
- 2- -
ClO2 + O  ClO3 -201.4
- 2- -
ClO3 + O  ClO4 -199.5

An alternative method is to ionize the aqueous calcium perchlorate molecule from reaction (1) with enough
ionizing radiation to directly break the ionic bound between the calcium and perchlorate molecules. This energy is
defined as the lattice energy. Since calcium perchlorate and magnesium perchlorate have theoretical lattice energies
of 1,958 kJ/mol and 2,268 kJ/mol, respectively [12], a high energy x-ray or gamma ray source would be able to
break down the compound. This would mitigate the need for recombination and still allow for the use of calcium
and magnesium that comprise the byproducts.

Another alternative is to implement the anion exchange process used in terrestrial perchlorate remediation in
groundwater sources [13]. This process exploits the fact that perchlorate compounds are highly soluble in water and
they are able to extract the perchlorate anion by switching it with one that is more reactive with water, such as a
harmless chlorine ion. A drawback to this method, and many others currently implemented in the terrestrial
environment, is the desire to only remediate the perchlorate content to levels below the toxicity threshold for
humans and not extract the perchlorate for potential applications.

Each method developed for perchlorate extraction will be subject to a full empirical analysis in future studies.
Because of the historical volcanic activity on Mars [15], it has been determined that soil samples from Mauna Kea
Volcano can be used as Martian regolith analogs [10]. These analogs will be the test subjects for each of the
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 methods developed. The next phase of the research will modify the newly develop perchlorate extraction methods to
operate on the Martian surface. With an atmosphere made up of mostly carbon dioxide at less than half the density
of Earth’s atmosphere and large temperature gradients over the course of a Martian sol [19], the system must be able
to survive extreme temperature fluctuations and intense levels of solar and cosmic radiation.

The resulting system is expected to have the ability to extract perchlorate from Martian regolith analog while
operating in the Martian environment conditions. The results will aid in future development of ISRU systems,
specifically in the realms of planetary resource utilization and rocket propellant. The development of a working
system to extract a specific material from the surface of another planet is expected to drastically decrease the amount
of shipped raw material needed during a space exploration mission.

III. Conventional and Alternative ISRU of Perchlorate Compounds

Prior to discussing potential uses for Martian perchlorates, it is worth noting that the capture of perchlorates
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serves an important purpose for manned missions to Mars. Perchlorates are recognized as a health hazard to humans
as it affects thyroid functions. As such environmental remediation on Earth is required when the perchlorate salts,
which are soluble in water, have contaminated the groundwater. The Southwestern United States is particularly
afflicted with this issue because of natural perchlorates in the soil and especially with the introduction of
perchlorates from the solid rocket motor manufacture and use [20].

In the case of Mars, the danger lies in the chemical contamination to astronauts through various means. Davila,
et al describes these as “direct inhalation of dust into the respiratory system, ingestion of contaminated water and
ingestion of foods grown in the presence of ClO4-” [21]. This same paper defines a biochemical process using
perchlorate reducing bacteria. In this way, “a daily supply of oxygen for one astronaut could be obtained by
complete dissociation of ClO4- contained in 60 kg of regolith” [21]. This exact topic of converting perchlorates to
usable oxygen warrants further discussion.

Beyond perchlorate remediation, a number of uses for in-situ Martian regolith perchlorate compounds are
proposed and discussed. A chief product of the perchlorates is in the production of oxygen. The discussion are then
divided between two categories: oxygen for human consumption and oxygen for propulsion.

As mentioned, elegant methods for extracting oxygen directly from the Martian carbon dioxide air exist. It is
worth noting that perchlorates in their solid form might prove a useful, albeit unconventional, oxygen reserve. A
prime example would be the use of Martian perchlorates in the production of oxygen candles. Oxygen candles rely
up on an exothermic reaction between (per)chlorates and certain fuels, contained in solid form and ignited to
produce a mass flow rate of filtered oxygen for human respiration. The most common application is in commercial
aircraft, specifically as the passenger oxygen reservoirs in aircraft. In an emergency, oxygen masks are deployed and
the pull of the masks from the overhead releases a firing pin that ignites the material, begins deflagration and starts
the production of oxygen. Other vehicle uses of oxygen candles include submarines, human spacecraft and space
stations. The latter maintains an inventory of oxygen candles in case the primary source (stripping oxygen via
electrolysis of water) is inoperable for any period of time.

It is useful then to cultivate the idea of oxygen candles as a means to produce in-situ oxygen at a moment’s
notice, especially in an emergency condition. Oxygen candles will be a necessity in this situation. Extended duration
missions will be required to manufacture or replenish these products from available Martian resources. The high
percentages of perchlorates found in the Martian regolith is a promising candidate for this solution, though certainly
other unique compounds are required. The large amount of readily available perchlorates opens up other
opportunities for mass production of oxygen. This premise can be extended to a larger scale whereas confined
oxygen farms harvest the perchlorate molecules with a byproduct of oxygen, either through exothermic reaction or
via the bioreactor described above. The use of perchlorates, specifically those most likely found on Mars, as
chemical oxygen generators is an area for further investigation.

Another proposed use for perchlorates is as a component in solid rocket motors. Terrestrial solid rocket motors
encompass four major constituents: an oxidizer, a fuel, a binder and a small amount of select additives. The majority
of the propellant mass is made of the oxidizer, usually ammonium perchlorate, AP, in nearly all solid rocket motors:

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 tactical, strategic and space launch vehicles alike. In the common composite ammonium perchlorate / aluminum /
HTPB formulas, which deflagrates at over 3,500°C, it is typical to have 70+ percent by mass of oxidizer.

Next, we extend the analysis to the use of Martian calcium perchlorate as the oxidizer using a common
aluminum fuel (AF), which can be harvested from the alumina (Al2O3) in the Martian regolith [22], and the most
common binder, hydroxyl terminated polybutadine (HTPB), as the constituents in a solid rocket motor propellant.
No additives are included for simplicity. These three combinations were run at varying percentages in the
thermochemical software ProPEP, which is a propellant performance evaluation program. Knowledge of the
stagnation temperature of combustion, the molecular mass and the ratio of specific heats for the combination of the
propellant products yields the total available enthalpy conversion and exhaust velocity of the propellant. This can
then be related to the specific impulse of the propellant, which is measured as the efficiency in which a mass of
propellant is converted to useable thrust impulse. For comparison to terrestrial values, an AP/AL/HTPB solid rocket
motor has a specific impulse of 260-265 seconds operating at 6.9 MPa (1,000 psi) with a nozzle expanded to an
ambient pressure at 0.101 MPa (14.7 psi) [1]. While a rocket motor operating on Mars would most certainly expand
the nozzle to a different, lower ambient pressure, these same chamber and exit conditions were maintained in the
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thermochemical evaluation of calcium perchlorate for ease of evaluation. Figure 1 is a ternary plot of the results,
showing a local maximum centered at a high oxidizer percentage ratio, as expected.

Figure 1: Thermochemical Ternary Plot of Calcium Perchlorate Oxidizer, Aluminum Fuel and HTPB Binder

The highest specific impulse combinations reveal an effective specific impulse of approximately 230 seconds,
again with a nozzle expanded to 0.101 MPa (14.7 psi). This is a reasonable agreement in terms of optimum ratio
between the three constituents as the AP/AL/HTPB blend, with 70-80% calcium perchlorate by mass having the
highest specific impulses in the range of 230 seconds. This underperforms the generic combination of AP/AL/HTPB
solid rocket motor which has a specific impulse of 260-265 seconds at the same conditions. However, because the
operation is intended for use on Mars only, which is a significantly different size than Earth, the smaller specific
impulse might still be sufficient to transport payload. The following example illustrates this concept.

According to the ideal ∆V equation, or total change in velocity attained for a rocket, the mass ratio for a single
stage rocket is given by ∆V = Ue * ln (mi/mf), where mi is the initial mass inclusive of propellant, and mf is the final
mass including the payload and any remaining structure. Ue is the exhaust velocity of the propellant which is related
to the specific impulse (Isp) by Ue = Isp * g0, where g0 is always set to Earth standard gravity (regardless of the local

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 gravity field the rocket motor is operating in, by convention). Staging will be ignored in this first example to make
use of the simplified ∆V equation.

On Earth, the total ∆V required to attain a circular low Earth orbit (LEO) is approximately 9 km/sec. This
includes not only the required change in velocity to maintain a circular orbit (7.78 km/sec at an orbit of 200km), but
also the ∆V penalties in the form of drag, gravity and steering losses. Launching Eastward with the rotation of Earth
effectively gains ∆V, the magnitude of which depends on the latitude of launch. A typical AP/AL/HTPB solid rocket
motor operating at an Isp of 260 seconds would then yield a mass ratio (mf/mi) of 0.029. In other words, this single
stage rocket would be filled 97% with solid propellant, the remainder of which, 3% of the total rocket mass, is
structure and payload. This is untenable as the current state of the art for mass fractions is just under 10% required
for structure and payload. A single stage solid rocket motor is unlikely to bring any appreciable payload to LEO
with current limits in specific impulse and structural mass fractions.

On Mars, the total ∆V required to attain a circular low Mars orbit is approximately 4.1 km/sec, largely owing to
the reduced 3.45 km/sec velocity required to reach a circular orbit of 200km. Using the calcium perchlorate single
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stage solid rocket motor operating at the lower Isp of 230 seconds (again, this is very conservative as the nozzle
expansion is severely suboptimal for this Mars condition), the rocket mass ratio would be 0.1624, meaning only
83.7% would be solid rocket motor propellant mass. The remaining 16.24% could be payload and necessary
structure. This is a very generous amount of payload for a simple single staged rocket to reach low Mars orbit.

Of course higher specific impulse propulsion systems yield exponential increases in the payload mass fraction
according to the ideal ∆V equation. A single stage liquid engine, methane and liquid oxygen being a popular choice
for Mars, might reach 350 seconds of Isp at Martian conditions, for a sizeable 30% for useable payload and structure
mass. This is at the expense of additional complexity of a liquid engine. Solid rocket motors are well known to be
safe, reliable and possess a long storage life and a quick response. Each variable must be weighed in turn according
to the desired mission profile. With that said, the above examples were explored for a single stage system. Staged
rockets increase the total ∆V substantially by jettisoning unused structural mass once the propellant is expelled from
that stage. For a fixed mass ratio of each stage using the same specific impulse, an increase in the number “n” of
stages directly increases the ∆V obtained according to ∆Vtotal = n*Ue * ln (mi/mf). That is to say, that two stages will
increase the total ∆V by a factor of two, three stages increase ∆V by a factor of three, and so on. There is a limit in
terms of diminishing returns with regards to the increase in complexity as a function of adding more stages; typical
space launch vehicles have two or three stages.

The addition of solid rocket motors that are fueled by Martian regolith perchlorates making up 70+ percent of
the mass of the propellant offers a new ISRU product to the collection of propulsion options. Other propulsion
systems can take advantage of this relatively free source of solid oxidizer. Extending the staging example further,
there are a plethora of staging combinations that can make use of solid rocket motors (simple solid rocket motor first
stage followed by a high performance smaller second stage, inexpensive reliable sacrificial or reusable strap-on
boosters, etc.). Beyond launch vehicles, staged combustion ramjets with solid grains can make use of the
perchlorates, not to mention defensive applications. Solid propellant divert attitude and control systems are also in
wide use, not to mention any number of devices that require pyrotechnics. Calcium perchlorate is also an ionic salt
which makes it a useable constituent in the new breed of electrically controlled solid rocket propellants with full
on/off/restart capability even at high operating chamber pressures [23].

There are a number of limitations to be explored in further research, such as suitable binders and native fuels
and additives. The question of combustion chambers, nozzles and associated subsystems has yet to be addressed.
However, these can most surely be overcome owing to the simplicity of these components. Certainly there are a
great many uses for a strong oxidizer, especially in the large quantities and ease of availability as found on the
surface of Mars. As a consequence of inevitable remediation of harmful perchlorates to the human anatomy, we
have the opportunity to utilize the resource in a number of beneficial applications.

IV. Summary & Conclusions

Mankind’s pursuit of space travel has net positive returns with regards to increasing the quality of life on Earth
and unearthing new technologies for commercial applications. It is fair to draw the same conclusions from our
continuing exploration of Mars. The existence of perchlorates on Mars presents unique challenges and opportunities.
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 The biohazard to astronauts is a known quantity which must be addressed. The knowledge we gain from remediation
in these activities can be further extended to life on Earth. The manner in which these perchlorates are remediated
can be further exploited to provide useful products on Mars. The literature review has identified a number of suitable
processes for this remediation. These include thermal decomposition and dehydration, ionizing radiation, anion
exchange process and use of bioreactors. Besides addressing necessary remediation of Martian perchlorates for
astronaut safety this paper also focuses on a number of potential uses including oxygen candles and solid rocket
motors. A few examples demonstrate the feasibility of such an approach. Future research is planned to develop
several such systems for perchlorate reclamation and ancillary studies using calcium perchlorate as an oxidizer for
solid propellant motors are also continuing.

Acknowledgments
B.F. Author thanks the Center for Space Nuclear Research (CSNR) and Idaho National Labs (INL) for funding
portions of this research. The authors acknowledge and thank colleagues Dr. Steve Howe, Mr. Ted Baker and Mr.
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Matthew Ralphs for contributions to the extended project.

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