RESEARCH ARTICLE
10.1029/2023JE007841
Key Points:
• Gas impermeable seals can form in
Mars‐like conditions in the soil with
5%–10% perchlorate salts by mass and
a shallow permafrost layer
• Methane could accumulate under the
seal in the shallow subsurface and be
released abruptly into the atmosphere
when the seal breaks
Supporting Information:
Supporting Information may be found in
the online version of this article.
Correspondence to:
A. A. Pavlov,
alexander.pavlov@nasa.gov
Citation:
Pavlov, A. A., Johnson, J., Garcia‐
Sanchez, R., Siguelnitzky, A., Johnson, C.,
Davis, J., et al. (2024). Formation and
stability of salty soil seals in Mars‐like
conditions. Implications for methane
variability on Mars. Journal of
Geophysical Research: Planets, 129,
e2023JE007841. https://doi.org/10.1029/
2023JE007841
Received 24 MAR 2023
Accepted 19 FEB 2024
Author Contributions:
Conceptualization: Alexander A. Pavlov,
Chris Johnson
Formal analysis: Raul Garcia‐Sanchez
Investigation: James Johnson,
Jeffrey Davis, Scott Guzewich
Methodology: Alexander A. Pavlov,
James Johnson, Ariel Siguelnitzky,
Jeffrey Davis
Resources: Ariel Siguelnitzky,
Chris Johnson
Supervision: Alexander A. Pavlov
Visualization: Raul Garcia‐Sanchez,
Prabhakar Misra
Writing – original draft: James Johnson,
Scott Guzewich
Writing – review & editing: Alexander
A. Pavlov, Prabhakar Misra
Published 2024. This article is a U.S.
Government work and is in the public
domain in the USA.
This is an open access article under the
terms of the Creative Commons
Attribution License, which permits use,
distribution and reproduction in any
medium, provided the original work is
properly cited.
PAVLOV ET AL.
Formation and Stability of Salty Soil Seals in Mars‐Like
Conditions. Implications for Methane Variability on Mars
Alexander A. Pavlov1 , James Johnson2 , Raul Garcia‐Sanchez3, Ariel Siguelnitzky1,
Chris Johnson4, Jeffrey Davis5 , Scott Guzewich1 , and Prabhakar Misra3
1
Planetary Environments Laboratory, NASA Goddard Space Flight Center, Greenbelt, MD, USA, 2Department of Civil
Engineering, Howard University, Washington, DC, USA, 3Department of Physics & Astronomy, Howard University,
Washington, DC, USA, 4NE‐L1division, Kennedy Space Center, Merrit Island, FL, USA, 5William H. Miller III
Department of Physics and Astronomy, Johns Hopkins University, Baltimore, MD, USA
Abstract Methane spikes observed in the Martian atmosphere require the abrupt release of large amounts
of methane from the Martian subsurface. The mechanism for such release has not been identified. We tested
whether gas traps can form under Mars‐like conditions in the shallow Martian regolith due to salt migration in
the icy soil. Experiments were performed on various soil samples in a Mars Simulation Chamber comprising
different perchlorate salts and water concentrations mixed with JSC Mars‐1A. Inside the chamber, the
samples were exposed to a range of temperatures from 20°C to 10°C and maintained CO2 gaseous pressure
between 8 and 10 mbars. As a methane analog, Neon was injected periodically underneath the soil sample. It
was found that over a wide range of Mars‐like soil parameters, a gas impermeable soil seal can form over a
relatively short period (3–13 days) but requires 5%–10% of perchlorate salt content in the soil. It was
determined that such a seal could sustain several mbars of neon above the Martian atmospheric pressure in the
soil. Based on our experiments, substantial amounts of gaseous methane may accumulate under the soil seal
and get released abruptly into the atmosphere upon seal cracking. An abrupt release of methane from the
shallow subsurface may help explain methane variability at the Martian surface, as the Mars Science
Laboratory detected.
Plain Language Summary Spikes of atmospheric methane on Mars, recently observed by the Mars
Science Laboratory mission, are puzzling. To explain rapid variations in methane abundance in the Martian
atmosphere, methane has to be released abruptly. Our experiments in the Mars simulation chamber
demonstrated that perchlorate salts can be transported toward the surface regolith via water migration and
subsequent sublimation. We showed that under Mars‐like conditions, the soil with migrated salts can become
cemented and form a solid gas impermeable seal. Methane and other volatiles can accumulate under the soil
seal. Methane seasonal variability and occasional methane spikes in the Gale crater on Mars can be due to a
sudden release of methane from the soil gas pockets when the Curiosity rover breaks soil seals by moving or
drilling.
1. Introduction
Atmospheric methane on Mars is of great interest because of its possible association with potential microbial
activity in the Martian subsurface. Besides microbial life, methane is a key molecular indicator of important
abiotic processes that might occur on Mars, namely Fischer‐Tropsch synthesis (Mumma et al., 2010) or degra-
dation of meteoritic organic matter (Keppler et al., 2012). All these processes could very well lead to methane
reservoirs in the Martian subsurface that are later released into the atmosphere.
All well‐established photochemical models state that the photochemical lifetime of methane in the Martian at-
mosphere is about 300–500 years (Atreya et al., 2007; Krasnopolsky et al., 2004; Summers et al., 2002). The
photochemical lifetime is much longer than the time of atmospheric mixing, suggesting that methane in the at-
mosphere would be evenly distributed over the planet and would not show change for many years (Summers
et al., 2002). Yet, several independent groups observed methane on Mars by both ground‐based telescopes and
Martian orbiters (Geminale et al., 2008; Krasnopolsky et al., 2004; Muma et al., 2009). Mumma's study reported
that methane column abundance exhibited both spatial and temporal variability at about ∼10 ppb levels. However,
those methane detections were challenged by Zahnle et al. (2011).
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In August 2012, the Mars Science Laboratory (MSL) Curiosity rover began
roaming on the surface of Mars in the Gale crater and continues to do so until
now. The Tunable Laser Spectrometer‐Sample Analysis at Mars (TLS‐SAM)
instrument on the Curiosity rover not only detected methane but also deter-
mined that its abundance is variable (Webster et al., 2014), sometimes
changing by up to 6 ppbv within a few sols (Martian days). Further TLS‐SAM
observations established that the average “background” methane abundance
of ∼0.4 ppb correlates with seasons. In the warmer spring and summer
months, methane abundances increase up to 0.65 ppb and decrease again
during the colder winter season to 0.24 ppb (Webster et al., 2018). In June
2019, TLS‐SAM detected a spike of 20.5 ppb of methane in the atmosphere,
even though only 1 ppb was detected earlier (Webster et al., 2021).

To add to the methane mystery on Mars, recent observations by the ExoMars

Trace Gas Orbiter (TGO) of the ExoMars mission did not detect any methane
above altitudes of 4–8 km (Knutsen et al., 2021; Korablev et al., 2019), even
though TLS‐SAM continued to detect methane at the ground level in the Gale
Figure 1. Concept of the soil seal formation and the migration of water and crater. There was an attempt to reconcile TLS‐SAM and TGO methane data
perchlorates. by proposing diurnal variations (Moores et al., 2019). Methane would
accumulate in the planetary boundary layer (PBL) at night when TLS‐SAM
conducts its measurements at the ground level. Then, methane would disperse during the daytime when PBL's
thickness increases and TGO makes its methane observations. Potentially, the diurnal methane variation
mechanism can “hide” the background (0.4 ppb) of methane from TGO. However, diurnal variations cannot
explain the detection of either occasional methane spikes or seasonal methane variability. Recent modeling
studies (Luo et al., 2021; Viudez‐Moreiras et al., 2021) agree that reconciling TGO and TLS‐SAM methane data
requires some local, small, unknown sources of methane within the Gale crater.
However, to explain rapid variations of methane abundance in the atmosphere (like the methane spikes or
methane seasonality in Webster et al. (2021)), methane has to be released abruptly rather than slowly and
gradually seeping from the deep interior (Oehler & Etiope, 2017). Not only does the methane‐release process have
to be abrupt but it also has to happen locally in the Gale crater. Moreover, the release of methane from the
subsurface has to be somewhat dependent on seasons. Such a process of methane release is currently unknown.
The Phoenix mission discovered permafrost just centimeters below the surface (Smith et al., 2009) and
perchlorate salts in the Martian regolith (Hecht et al., 2009). Other salts are also present in the Martian regolith
(Clark & Van Hart, 1981; Thomas et al., 2019). The Curiosity rover confirmed the ubiquitous presence of
perchlorate salts in the Martian subsurface (Kral et al., 2016).
The presence of perchlorates and shallow ice points to the possibility of some amount of mobile water in the
shallow Martian subsurface due to the low eutectic point of perchlorates. Under low‐pressure conditions, water
can migrate to the surface and evaporate once it reaches the top. With the presence of salts in the ground, some
salts are inevitably dissolved in the water and transported to the surface via water migration (see Figure 1).
Once most of the water evaporates or ice sublimates, hydrated salts are left in the top few centimeters of the
soil. We hypothesize that the soil with migrated salts can become cemented similar to the terrestrial duricrust
(Lewinger et al., 2018; Miller, Hibbitts, & Mellon, 2020; Miller, Mellon, et al., 2020), and form a solid seal
barrier capable of trapping volatiles underneath. Under such soil seals, methane gas, regardless of its origin, can
accumulate. If those areas are disturbed (e.g., impacts, seasonal temperature variations, or motion of the
rover itself), then methane can be released abruptly into the atmosphere. Our laboratory experiments aimed to
test the formation, strength, and stability of salty soil seals formed under Mars‐like (pressure, temperature)
conditions.

2. Materials and Methods

Mars‐like simulations of the shallow permafrost layer were performed using a Mars Simulation Chamber
(Figures 2a–2c). In this section, we describe the general structure of the Chamber (Section 2.1), sample holder
details (Section 2.2), sample preparation procedure (Section 2.3), and experimental run procedure (Section 2.4).

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Figure 2. (a) Mars Simulation Chamber, (b) a close‐up of the sample in the sample holder in the chamber, (c) block diagram
of the entire setup. The Chamber could reach temperatures below 100°C and pressures down to as low as 0.1 mbar.

2.1. Chamber Description

The Martian Simulation Chamber (Figure 2a) is made up of a glass dome that sits on top of a cylindrical steel
housing. The chamber was connected to a vacuum pump capable of pumping down the chamber pressure to as low
as 0.1 mbar, which created a vacuum seal between the dome and housing. Figure 2b shows a close‐up view of the
sample in the chamber. Above the sample holder, there was an aluminum foil dome which had a light source and a
camera. The pump evacuated air from the chamber and beneath the sample (Figure 2c) and used valves 3, 5, and 6
to control which area was pumped down. Between the pump and the chamber sat a moisture collection system that
used the low temperature of liquid nitrogen to condense and trap water before it entered the pump. The moisture
collection system was used only during short periods in the run when there was high moisture content coming off
the soil sample inside the chamber (usually at the beginning of the run). Inside the chamber sat another smaller
cylindrical metal housing (Figure 2c) in which the sample holder was placed. During experimental runs, CO2 was

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continuously injected into the chamber through valve 7 (Figure 2c) and
pumped down from the chamber at the same time through the valve 6
(Figure 2c). Such a flow‐through system allowed the setting of the desired
CO2 pressure in the chamber above the soil sample. The chamber's CO2‐flow‐
through system also ensured that water vapor from the sample was steadily
removed from the chamber. However, at present, there is no humidity sensor
in the chamber. Before each experimental run, the entire system was pumped
down and purged with nitrogen gas through valve 2.
The sample holder was placed on the cold plate and inside the metal housing
(Figure 2b) with an open top. A solenoid valve was used to control the flow of
liquid nitrogen through the cold line, which went through the cold plate
(Figure 2c). Therefore, by adjusting the solenoid valve, it was possible to
control the temperature of the sample and to bring sample temperatures as low
as 100°C (Figure 2c). The chamber setup had the option to change the
surface temperature by using the light source located in the aluminum foil
Figure 3. Diagram of the side profile of the sample holder with a typical dome (Figure 2b), but the light source was not used in this study. Several
sample inside. thermocouples were used to monitor the temperature of the cold plate, sample
holder housing, cold line temperature, and the gas temperature in the cham-
ber. Baratron 1 was used to measure the pressure inside the capillary tube beneath the sample and Baratron 2 was
used to measure the pressure inside the chamber above the sample (Figure 2c). The chamber had a separate
capillary tube that was connected to a mass spectrometer (not used in this study). The soil sample was placed in a
sample holder (Figure 3).

2.2. Sample Holder Description

The sample holder was a thin stainless steel cylinder that sat on the cold trap plate and was inside the larger
cylindrical metal housing (Figure 2b) inside the chamber. The sample holder was 6.7 cm in internal diameter
and 9.5 cm in depth. To have better contact between the sample material and the metal walls, the sample holder
was built with ridges and grooves that started about halfway up the holder and continued to the top (see also
Figures S3 and S4 in Supporting Information S1). Ridges and groves provided a longer path for volatile
molecules to move along the metal wall of the sample holder. Thus, if a microcrack between the steel wall and
the frozen soil developed at some depth, there was still sufficient soil column mass along the wall to seal
volatiles in the soil. Inside the holder, there were two thermocouples—one that extended 2 cm up from the
bottom to measure the temperature of the bottom of the sample and another that extended 6 cm from the bottom
to measure the temperature of the upper part of the sample (∼2 cm below the top of a sample's soil level).
Thermocouples could measure temperatures with an accuracy of 0.01°C. In this study, the only relevant
temperature readings were from the top thermocouple because salty soil seals were formed toward the top of
the sample. In the middle of the sample holder, a capillary tube extended 3 cm up from the bottom of the
holder. The capillary tube was connected to the neon tank and had a 0.13‐mm hole at the top to inject the neon
beneath the sample.

2.3. Sample Preparation Procedure

Depending on the experiment, samples of different salt and water concentrations were mixed with JSC
Mars‐1A. JSC Mars‐1A is the Martian regolith analog due to its similar porosity and bulk density to soil
found at the Viking landing site on Mars (Seiferlin et al., 2008). Before each experiment, JSC Mars‐1A was
washed with deionized (DI) water for at least five consecutive times to remove any residual salt from
previous experiments. The “desalted” JSC Mars‐1A sample was then placed in a small pan and dried in the
oven at +70°C for at least 20 hr to remove the introduced moisture. Dry and desalted JSC Mars‐1A was
then mixed with DI water or a solution of DI water and salts. The salt concentration was reported in Msalt/
(Mdry soil + Msalt) % (see Text S1 in Supporting Information S1). Salt was dissolved in DI water at room
temperature before mixing with soil. For the consistency of various experimental runs, it was important to
ensure a uniform salt distribution in the soil sample before the experiment. We determined that JSC Mars‐
1A became completely saturated with water at Mwater/(Mdry soil + Mwater) ∼35%–37% by weight. Therefore,
the initial water content at 40% by weight was kept for all permafrost samples. After mixing, the salty soil‐

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water mixture was poured into a sample holder (Figure 3) and placed in the freezer ( 20°C) overnight for
at least 15 hr (see Figure S1 in Supporting Information S1). After the sample was completely frozen, it was
placed in the Mars Simulation chamber for an experimental run.

The samples were then placed in the Mars Simulation Chamber. Inside the chamber, samples were exposed to a
range of temperatures from 20°C to +5°C and the chamber pressure was kept between 8 and 10 mbars. 2–
5 mbars of neon were injected periodically beneath the sample. Neon was used as an analog to methane because it
had a similar molecular weight to methane. Like methane, neon was not reactive with soil and had a similar
diffusivity in water. Therefore, neon was expected to diffuse similarly to methane in the soil, but neon was much
safer to work with in the laboratory.

2.4. Experimental Run Procedure

Before each experimental run, the sample holder, the cold plate, and the capillary inlet were cleaned with ethanol
to remove any residual salt crystals or dust particles from previous runs. The empty chamber was then pumped
down to ∼1–5 mbar at room temperature and kept at low pressure for at least 12 hr to remove the residual moisture
from previous runs. Each time during placement of the sample holder into the chamber a new copper washer was
used to connect the capillary tube (Figure 2b) and its flex line and then tightly screwed the two together. The
thermocouples on the sample holder were connected to their corresponding connectors in the chamber. Ethanol
was used to carefully clean the points of contact between the rubber on the base of the glass dome and the metal
housing on the chamber (Figure 2b).
After the sample holder with a sample was placed in the chamber, each experimental run followed the following
steps:

1. The glass dome was placed on the metal housing and the chamber was pumped from above the sample
by opening valve 6 (chamber) and beneath the sample by opening valves 3 and 5 (capillary tube) (See
Figure 2b).
2. The solenoid connected to the liquid nitrogen cold line was set to 90°C to allow the chamber to cool quickly
and for a sample to remain ∼ 20°C.
3. Once the chamber pressure decreased to ∼10 mbar, valve 3 (Figure 2b), which pumps from the capillary tube,
was closed and allowed the volume below the sample to equilibrate with the rest of the chamber. The chamber
pressure gradually decreased down to 0.3–1 mbar due to constant pumping from the chamber through open
valve 6.
4. Then, using valve 7 (See Figure 2b), CO2 was injected slowly into the chamber to increase the chamber
pressure to the desired CO2 level (between 8 and 10 mbars) while continuing constant pumping from the
chamber through open valve 6 (see Section 2.1).
5. The solenoid's setting was adjusted to get the sample to its desired temperature.
6. Once temperature and pressure in the chamber and the capillary tube were equilibrated and stabilized, be-
tween 3 and 5 mbars of neon (measured with Baratron 1) were injected directly into the capillary tube using
valve 1, and the evolution of pressure in the capillary tube was recorded. If the Pcapillary remained elevated
compared to the Pchamber, it was considered that a seal had formed.
7. If a seal had formed, then the temperature of the soil was raised to >0°C to determine the stability of the seal
at higher temperatures (up to +5°C). Note that once the seal was formed, the capillary tube was isolated from
the chamber gases. Thus, the background gas in the “isolated” capillary tube was the water vapor from the soil
below the seal as opposed to the chamber's CO2/H2O gas mixture. Therefore, the background pressure in the
capillary tube could be a function of soil temperature and soil water abundance.
8. The duration of the experimental run depended on the stability of the seal. If a seal was formed (typically
within 1–2 days), the run could continue for several days or weeks. The soil temperature and pressure were
recorded every 5 s during neon injections and shortly thereafter.
9. If a seal was not formed within 1–2 days from the experiment's start, then the temperature of the sample was
increased. Sometimes temperature increases result in seal formation, but prolonged exposure to higher
temperatures (>0°C) eventually breaks soil seals.
10. Once the seal was broken, then the experiment was stopped, and the sample was removed from the chamber
within 24 hr. No long‐duration experiments on the potential seal reformation were conducted.

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Table 1
Summary of the Samples Tested for Gas Permeability
Number of Temperature range Chamber Seal
Experiment repetitions Description (top thermocouple) pressure Seal duration
1 2 100% Water 2°C to 3°C 8 mbar No N/A
0% Mg(ClO4)2
(Pure Ice) (Sample 1)
2 2 40% Water; 60% JSC Mars‐1A; 0% Mg(ClO4)2 (Pure Permafrost) (Sample 2) 12°C 8 mbar No N/A
3 3 40% Water; 50% JSC Mars‐1A; 10%Mg(ClO4)2 Permafrost (Sample 3) 15°C–5°C 8–10 mbar Yes 12 days
4 3 40% Water; 55% JSC Mars‐1A; 5% Mg(ClO4)2 Permafrost (Sample 4) 15°C–5°C 8–10 mbar Yes 19 hr
5 2 40% Water; 58% JSC Mars‐1A; 2% Mg(ClO4)2 Permafrost (Sample 5) 15°C–5°C 8–10 mbars No N/A

3. Results
Table 1 provides a summary of the experimental runs in our study. The formation of soil seals was observed in
both salt‐icy soil mixtures. Samples with pure ice and pure permafrost did not exhibit gas‐impermeable seal
formation.

3.1. Non‐Salt Samples

Intuitively, pure ice as a solid body should be gas‐impermeable. To confirm
that our first experimental run was to test the gas permeability of the pure ice in
the Mars Simulation Chamber (Figure 2b). Figure 4a shows the results from a
sample of frozen deionized water. The sample was placed in the chamber and
maintained at 2°C to 3°C. After temperature and pressure stabilized, 3 mbar
of neon was injected beneath the sample. The pressure beneath the sample
quickly equilibrated with the rest of the chamber (Pcapillary = Pchamber), which
meant that pure ice was not able to trap neon beneath. Our results indicated that
pure deionized ice samples developed microcracks, allowing rapid neon
escape into the chamber.
As demonstrated by the Phoenix mission, shallow permafrost is abundant at
Mars high and mid‐latitudes (Piqueux et al., 2019). Therefore, our next run was
focused on permafrost gas permeability. Figure 4b shows the results from a
sample consisting of JSC Mars‐1A and 40% deionized water. The sample was
placed in a freezer overnight (at 20°C) and then placed inside the chamber. In
the chamber, the sample was kept at 12°C, and the chamber pressure was
maintained at ∼8 mbars. The pressure immediately equilibrated when 3 mbar
of neon was injected beneath the sample. We continued the run, periodically
injecting neon to see if a seal would form, but repetitive neon injections did not
result in any gas accumulation below the permafrost (Pcapillary = Pchamber). The
sample was kept for 52 hr total in the chamber. Based on the observed pressure
equilibration, the pure JSC Mars‐1A permafrost without the presence of salts
also developed microcracks and could not form a nonpermeable gas seal.

3.2. Samples With Perchlorate Salt

In the next runs, permafrost samples with Mg‐perchlorate salts were studied.

3.2.1. 10% Mg(ClO4)2, Initially Uniform Permafrost

Figure 4. (a) Pure ice sample (Sample 1, Table 1). Neon injections showed
immediate pressure equilibration. Temperature at 2°C to 3°C (top
thermocouple [see Figure 3] reading in all Figures). (b) Pure permafrost
(Sample 2, Table 1) no salt. Neon injections showed immediate pressure
equilibration. The temperature of the sample was kept at ∼ 12°C.
Figures 5a–5d show the results from Sample 3 (Table 1), which contained
10% Mg(ClO4)2 and 40% deionized water frozen into permafrost (Figure S4
in Supporting Information S1). During the first day in the chamber
(Figure 5a), the seal formation was not observed—capillary tube pressure re‐

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Figure 5. Various neon injections into 10% Mg(ClO4)2 permafrost before, during, and after seal formation (Sample 3, Table 1). (a) The temperature was kept at 7.5°C.
Neons were injected 26 hr after being placed in the chamber. “Capillary Tube Pumped Down” means pumping down the capillary tube itself and the sample's soil matrix
from below. (b) 3 mbar neon injection showing a stable 25–hr long seal. The temperature was kept between 14.5°C and 12.5°C. Neon was injected 8 days after being
placed in the chamber. (c) 66‐hr seal also shows pressure decrease until reaching seal limit. The temperature was kept between 14.5°C and 11.5°C. Neon was injected
after 9 days in the chamber. (d) Stable 25‐hr seal below seal limit. The temperature was kept between 6°C and 3°C. Neon was injected after 13 days in the chamber.
(e) Seal break. The temperature was maintained at ∼+2.5°C for about 20 hr before breaking. Neon was injected after 16 days in the chamber.

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equilibrated quickly after neon injections (Pcapillary = Pchamber). It was verified

that gas diffused through the soil both ways. During the “Capillary Tube
Pumped Down” event (Figure 5a), we deliberately brought the capillary tube
pressure below the chamber's pressure. Since there was no seal in the soil at
the beginning of the run, CO2 from the chamber above the sample quickly
diffused through the soil into the capillary tube and pressures re‐equilibrated
(Pcapillary = Pchamber).
Pressure equilibration between the chamber and capillary tube occurred
within 5 s after the neon injection. Over the next few days (not shown), there
were signs of a possible incomplete seal formation—the capillary tube
pressure still equilibrated with the chamber pressure, but over increasingly
longer periods. After the fourth day in the chamber, a seal formation was
observed with persistent Pcapillary > Pchamber. It was established that the salty
soil seal could hold 3–4 mbars of additional neon pressure. However, there
Figure 6. (a) Sample 3 (Table 1) directly after the sample run. (b) Salt was a limit to how much pressure could be held beneath the seal.
cemented soil layer carefully removed from the top of the sample. Upon
removal from the chamber, the solid soil layer absorbed atmospheric water Figure 5b shows a stable seal after ∼8 days in the chamber (hour 187 of the
vapor and softened in about 10 min. experimental run). It was verified that the formed seal is gas impermeable
from both directions. Specifically, during the “Capillary Tube Pumped
Down” event (Figure 5b), the gas was pumped down from the capillary tube itself and the sample's soil matrix
from below. However, since there was a seal in the soil, CO2 from the chamber could not diffuse through the soil
down to the capillary tube and Pcapillary remained lower than Pchamber after pumping stopped. This was proof that
the soil seal was impermeable to both neon (injections from below) and CO2 (lack of equilibration after capillary
tube pumping) in both directions. In subsequent “Capillary Tube Pumped Down” events (Figures 5c and 5d), the
pumping of the capillary tube was stopped when the capillary tube pressure was about equal to the chamber's
pressure.

The seal was able to withstand 3 mbars of neon gas pressure differential between the capillary tube and the
chamber (Pcapillary–Pchamber ∼ 3 mbars). However, when a larger neon injection was made after 9 days of being in
the chamber (hour 217, Figure 5c) and 7 mbars of pressure differential was established, the neon slowly leaked
until the pressure differential decreased down to ∼3.5 mbars. After ∼13 days in the chamber (hour 306,
Figure 5d), the soil seal's stability was tested again under higher temperatures (Figure 5d). The temperatures were
kept between 6°C and 3°C. Just as in the pure ice and pure permafrost runs, the vertical temperature gradient
between the top and the bottom thermocouples was <1°C. Figure 5d validates that the seal can hold ∼3.5 mbars
pressure differential even if the temperature of the soil varies from 6°C to 3°C for over 25 hr. As shown in
Figure 5e, once the sample reached the temperature of about +2.5°C and was held at that value for ∼20 hr, the seal
broke, and the neon was released. In total, soil seals were observed during a total of 12 days: 16th day (seal break)
—4th day (first observed seal) = 12 days. Over those 12 days, seals were tested under multiple temperatures,
starting at 14°C and slowly increasing to +5°C and multiple capillary tube pressures. We were not able to
reform the seal in Sample 3 by decreasing the temperature to below freezing once the seal was broken. Further
comprehensive studies are needed on the possibility of soil seal “reformation.” 10% Mg(ClO4)2 permafrost
experiment has been repeated 3 times (Table 1). Soil seals formed consistently in all three repetitions within 3–
5 days from the start of each run.
Figures 6a and 6b demonstrate Sample 3 after the run. A soil seal was extracted from Sample 3 after 19 days in the
chamber (Figure 6b). The soil seal was solid and about 1 cm thick. The seal absorbs atmospheric water over time
outside the chamber, and the soil becomes noticeably wet and breakable. Sporadic salt crystals can be seen in the
soil seal with the naked eye (Figure 6b).

3.2.2. 5% Mg(ClO4)2 Initially Uniform Permafrost

After the soil seal formation was observed in the sample with 10% Mg perchlorate, we decided to test whether a
seal could form at a lower perchlorate soil concentration. Therefore, in the next run (Sample 4, Table 1), a
permafrost sample with the perchlorate abundance at 5% by weight (Figure S5a in Supporting Information S1)
was prepared. Similar to the 10% perchlorate sample, the 5% perchlorate sample also did not show seal formation
at the start of the experiment (Figure 7a). Sample 4 was tested with 3–5 mbar injections of neon at 13°C, 12°C,

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10°C, 7°C, 5°C, and 2.5°C. Only after the sample temperature (top
thermocouple Figure 3) was raised to 1.7C, a decrease in neon diffusion
through the soil sample was observed (Figure 7b).

Figures 7a, 7b, and 7c show the results for Sample 4, which contains 5% Mg
(ClO4)2 and 40% deionized water frozen into permafrost. Soil seal formation
(Pcapillary = Pchamber) was not observed for the first 2 days (Figure 7a).
However, the equilibration times started at ∼5 s, but after 48 hr of being in the
chamber and raising the temperature from 14°C to 1.75°C, the equili-
bration time increased to ∼10 min, as shown in Figure 7b. An equilibration
time increase indicates that a seal has started to form. Once the sample
reached ∼ 1°C, a clear sign of seal formation (Pcapillary > Pchamber)
(Figure 7c) was observed. We continued to increase the soil temperature up to
∼+1°C, but the seal lasted for 19 hr before breaking (Figure 7c). No attempt
was made to reform the soil seal by decreasing the temperature afterward. 5%
Mg(ClO4)2 permafrost experiment has been repeated 3 times (Table 1). Soil
seals formed consistently in all three repetitions within 2–3 days from the start
of each run when temperatures of the samples were brought up to 2°C, 1°
C. We did not explore the possibility of soil seal formation at lower tem-
peratures for 5% Mg(ClO4)2 permafrost runs.
In a separate 5% Mg(ClO4)2 permafrost run (not listed in Table 1), the seal
formation was observed after 70 hr since the start of the run. The experiment
was conducted under 10°C sample temperature and 8–10 mbars chamber
pressure. After 92 hr since the start of the run, we accidentally brought
(Pcapillary–Pchamber) pressure differential under the soil seal in a significant
excess of 5 mbars. That soil pressure spike resulted in an explosive breakup of
the soil seal—a piece of the cemented soil was blown away from the sample
(Figure S4 in Supporting Information S1). Unfortunately, the exact soil
pressure differential for the explosion was not recorded digitally but it was
observed by the chamber operator to be ∼10–15 mbars. The run was stopped
shortly after the explosion for chamber cleanup. No intentional attempts to
reproduce the explosion in the chamber were made.
In a separate 10% Mg(ClO4)2 permafrost experiment (one of the repetitions
for Sample 3, Table 1), a short‐duration test was made on the stability of the
soil seal to colder temperatures. Conditions of seal formation described in
Figure 5b were maintained (∼ 15°C sample temperature, 8–10 mbars
chamber pressure). Shortly after the formation of the soil seal, the sample
temperature was rapidly dropped to 30°C and then down to 40°C. The soil
seal's gas permeability was tested at both temperatures by injecting 3 mbars of
neon. Each pressure test injection was done for 1 hr. At both temperatures, the
seal was holding 3 mbars of excess pressure. The run was stopped after the
40°C seal permeability test without breaking the seal.

4. Discussion
4.1. Limitations, Assumptions, and Future Experimental Studies
In our study, the evidence of the soil seal formation was based on measuring
Figure 7. (a) 5% Mg(ClO4)2 permafrost before seal formation (Sample 4,
Table 1). Temperature: 7°C. Neon injected after 25 hr in the chamber. the gas pressure in the chamber above the soil and comparing it to the pressure
(b) 5% Mg(ClO4)2 permafrost 10 min equilibration. Temperature at 1.7°C. in the capillary tube below the soil sample (Figure 3). If after injection of neon
Neon injected after 48 hr in the chamber. (c) 5% Mg(ClO4)2 Permafrost 19‐ Pcapillary remained elevated compared to the Pchamber, it was considered that a
hr seal and seal break. The temperature was at 1°C (50 hr in the chamber). soil seal had formed. As shown in Figure 6b, it was sometimes possible to
extract the salt‐cemented soil layer relatively intact after the end of the run.
However, our setup did not have a third pressure sensor inserted in the middle of the soil. Therefore, a potential
question might be raised whether the neon gas blockage could occur at the point of neon injection into the soil at

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the tip of the capillary tube (see Figure 3) rather than at the top of the sample in the salt cemented soil layer. Note
that the tip of the capillary tube was only 0.13 mm, while the internal diameter of the soil sample holder at the top
opening was ∼7 cm (Figure 3).

There are two reasons why the salt‐cemented soil layer (Figure 6b) had to be gas‐impermeable to explain the
observed data (Figures 4, 5, and 7) regardless of whether the tip of the capillary tube was plugged at any point.
First, all experimental runs presented in Table 1 started without a detectable soil seal (see Figures 4a, 4b, 5a,
and 7a). Therefore, pure ice, pure uniform icy permafrost, and uniform icy permafrost with perchlorate samples
were all gas‐permeable. Hence, the 0.13 mm tip of the capillary tube frozen into those icy matrices had to be
gas‐permeable as well. When the seal formed (e.g., Figure 5b, ∼1 week in the chamber), the temperature of the
entire sample temperature was maintained in the range of 14.5 12.5°C. Therefore, the capillary tube was
clogged with the same salty icy permafrost as at the beginning of the run. The only difference in the sample
structure, compared with the starting conditions, occurred in the top ∼2 cm of the sample, where the ice
sublimated to the chamber (due to low chamber pressure) and salt accumulated cementing the topsoil layer.
Thus, the pressure differential observed in Figure 5b was consistent only with the gas‐impermeable cemented
topsoil layer.

The other evidence that the seal must occur in the cemented soil layer came from the “explosion” run shown in
Figure S4 in Supporting Information S1. If the seal were to occur only at the 0.13 mm opening of the capillary tube
while the soil cemented layer would be gas permeable then there was no feasible way to build up enough pressure
in the soil to cause the explosion and lift of a chunk of cemented soil. At 10 mbar neon pressure, a capillary tube
with an opening of 0.13 mm would generate an upward force of only ∼10 5 N, which is at least 2000 times
smaller than the force necessary to lift 1 cm3 of cemented soil (see Figure S4 in Supporting Information S1). The
only way to lift several grams of soil is to accumulate critical pressure inside the soil under the gas‐impermeable
soil seal.
Several planetary parameters can affect soil seal formation on Mars, which were not studied in our chamber
simulations. For example, as stated in Section 2.1, the CO2‐flow‐through system constantly removed water vapor
from the chamber, but relative humidity above the soil was not measured. In theory, if the air above the soil is dry,
then the sublimation rate from the sample should increase. Thus, the rate of salt‐cemented soil formation on Mars
could be more effective.
Lower gravity would result in easier vertical diffusion of the salty water toward the top of the soil. Thus, the rate of
soil seal formation might be faster on Mars under the same pressure/temperature conditions.
We discovered the formation of gas‐impermeable soil seals in soil samples with Mg(ClO4)2 perchlorate salt
abundances of 5%–10% under Mars‐like pressure/temperature conditions (Figure S2 in Supporting Informa-
tion S1). A regolith salt abundance of 5%–10% by weight is consistent with some locations on Mars reported by
Wray et al. (2011). Using thermal emission spectra of minerals (e.g., gypsum, hydrated Mg/Fe‐sulfates, and
kaolinite), they found that in the Columbus crater in the Terra Sirenum region of Mars, salt abundances are in the
tens of percent range. Overall, the Phoenix lander mission and MSL reported 0.5%–1% of perchlorates wide-
spread in Martian soils and regolith. However, some areas in the Martian regolith have concentrated amounts of
salt (Fergason et al., 2006; Golombek et al., 2006; Hurowitz & Fischer, 2014; Wang et al., 2008).
Several experiments were conducted with 2% perchlorate permafrost samples (Sample 5, Table 1). In all low‐salt
experiments, the formation of isolated soil clumps was noticed but not a gas‐impermeable layer of soil (Figure S3
in Supporting Information S1). However, laboratory experiments are limited to several weeks and may not
capture the effect of seal formation at lower salt abundances. On Mars, such a process can occur naturally over a
long period of time in the shallow permafrost regions, and it may be possible for enough salt to accumulate in the
top layer to form a seal, even if the average abundance of salt in regolith is lower. Further long‐duration ex-
periments are needed to determine the salt‐abundance threshold for seal formation. Also, our experiments should
be conducted for sulfates, given their high abundance on Mars.
The exact concentration of Mg(ClO4)2 perchlorate salt in the solid seal was not measured in our experiment.
However, upon extraction from the chamber, salt crystals (Figure 6b) can be clearly seen filling the soil pores in
the solid soil seal layer, suggesting the upward transfer of salt by evaporating water during the experimental run.
Once the impermeable gas seal forms, methane from any biological or abiotic source can accumulate under the
seal.

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During the 10% Mg(ClO4)2 permafrost run, we noticed a limit in the amount of pressure the seal could hold.
Figure 5c shows that if the excess pressure under the seal is ∼5 mbar, neon starts seeping through the seal, but
∼3 mbar of excess neon pressure is stable under the seal (Figures 5b and 5d). This phenomenon was consistent
throughout the entire run under multiple injections at different temperatures. In the 5% Mg(ClO4)2 permafrost run
(Sample 4), soil seal stability was not tested and neon injections were kept at ∼3–3.5 mbar only (Figure 7c).
Therefore, future studies need to explore the dependence of the seal‐breaking pressure threshold on salt abun-
dance in the soil.
The soil seals for perchlorate soil mixtures were found to be stable over a wide range of temperatures and had a
fairly strong stone‐like appearance (Figure 6b). Not only were the soil seals able to hold ∼3 mbar of pressure
differential (neon excess pressure) beneath, but they were able to do it repeatedly. Most of our neon injections
were ∼3 mbar, and the soil seals, once established, would hold such pressure excess indefinitely in all our ex-
periments as long as the sample temperatures remained below 0°C (top thermocouple [see Figure 3]). When the
soil temperatures were increased above 0°C, the soil seals did not break immediately. It took hours (Figure 7c) of
continuous soil temperatures >0°C to break the seals formed in soils with 5%–10% salt abundance by weight. We
hypothesize that the prolonged increase in the soil temperature above 0°C allows the water in the seal layer to
evaporate, and eventually, the water content decreases to a point where microcracks appear in the soil, causing the
seal to lose its gas impermeability.
All experimental runs that resulted in the formation of soil seals were started from uniform salty‐permafrost
samples (Figure S1 in Supporting Information S1). As ice rapidly sublimated due to low Martian‐like chamber
gas pressure above the sample, water with salt migrated toward the top layer of the sample, and an ice‐free soil
seal formed at the top of the sample (Figures 6a and 6b; Figure S2 in Supporting Information S1). This type of
process might occur at present in shallow permafrost regions at high and mid‐latitudes on Mars where shallow
permafrost and ice are present (Dundas et al., 2021; Piqueux et al., 2019). However, further experiments are
needed to determine the timescale of seal formation at lower temperatures. We observed soil seal formation in
salty permafrost at temperatures 14.5°C 12.5°C (Figure 5b). Martian surface temperatures at high and mid‐
latitudes are substantially lower. Lower temperatures would most likely result in significantly longer times to
develop salt‐cemented soil seals due to the lower mobility of salts.

At low latitudes (e.g., Gale crater), the temperatures of the surface and shallow subsurface (Martin‐Torres
et al., 2015) overlap with the temperature range in our experiments. However, there were no reports of permafrost
in the Gale crater, and thus, no active formation of soil seals is expected at present. Salt‐cemented soil seals could
have formed at low latitudes and equatorial regions (specifically in the Gale crater) at the end of a period of high
obliquity (e.g., Emmett et al., 2020; Levrard et al., 2004) when ice and permafrost were abundant at low latitudes.
As ice started to sublimate and retreat to the poles, salt‐cemented soil seals would form. Once soil seals are formed
and buried by even a couple of centimeters of loose soil, the seal becomes sufficiently isolated from surface
temperatures and can survive indefinitely.

4.2. Relating Experiments to Mars Methane Observations

To relate our gas trap stability experiments to Mars' shallow subsurface, we used the MarsWRF general circu-
lation model output of the subsurface temperature at 2 cm depth, which is also the soil depth at which the
temperature readings in our experiments were reported (top thermocouple, Figure 3). MarsWRF is the Mars‐
specific version of the PlanetWRF general circulation model (GCM) (Richardson et al., 2007; Toigo
et al., 2012). We used a 5° horizontal resolution simulation with prescribed dust corresponding to the Mars
Climate Database Mars Global Surveyor scenario (Montmessin et al., 2004) and correlated‐k radiative transfer as
described by Mischna et al. (2012). The simulation was run for four Mars years with hourly output, with Figures 8
and 9 representing average temperatures across that duration. MarsWRF model temperatures on 15 subsurface
soil layers, and the surface skin temperature. Soil temperatures were modeled through subsurface heat conduction
parameterization and sensible heat exchange with the surface layer (Toigo et al., 2012). MarsWRF assumed a
constant heat capacity in the soil of 837.2 J/kg/K, representing a reasonable average value for basalt‐dominated
regolith. It used thermal inertia from Thermal Emission Spectrometer measurements (e.g., Christensen
et al., 2001) to calculate thermal conductivity. The near‐surface soil density was set to 1,500 kg/m3 (Shorthill
et al., 1976). Our experiments determined that prolonged exposure (several days) of a salt soil seal to temperatures

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above 273 K usually results in seal breaking. This experimentally observed

quality of soil seals can be used to estimate their global stability.

Figure 8 shows that the temperature at 2 cm depth never exceeds the freezing
point of water over most of the Martian surface (gray area). That means that
over the vast majority of the Martian surface, the salt soil seals would remain
stable, and any methane from the subsurface, produced by either abiotic or
biological sources, can accumulate under such seals for a long time.

Surprisingly, Gale Crater is located right on the edge of the area where the salt
soil seal can become unstable. Therefore, methane detection within Gale
Crater during the warmer months of a Martian year (Webster et al., 2018) is
consistent with the breaking of salt seals in Gale and the local release of
Figure 8. Total hours per year when the temperature exceeds 273K at 2 cm methane.
depth. The gray color represents a permanently frozen area at 2 cm depth. A
narrow band between the edge of the gray area and a 100‐hr contour line
The potential link between seasonal variations in methane and shallow sub-
represents an area where soil temperature exceeds 273 K at 2 cm for 0– surface temperatures is demonstrated in Figure 9. It is noteworthy that the
100 hr. Gale crater (black star) is right on the edge of that band, and therefore lowest background levels of methane were observed during the Northern
soil seals can be less stable. The central band (between 100‐hr contours) Spring, which is the season when salt soil seals are the most stable due to
represents an area on the Martian surface where salt soil seals would likely lower temperatures and the most effective at trapping methane.
be unstable yearly.
Figure 9 shows that the maximum soil temperatures do not quite reach 273 K
at 2 cm depths but can exceed the freezing point of water at 0.5 cm depths during the Northern Hemisphere
Autumn in Gale. However, it should be re‐emphasized that Figure 9 was generated using the output of MarsWRF
with a 5° horizontal resolution simulation. Therefore, the model does not fully resolve the local topography,
specifically the low elevation at the Curiosity rover location. Accounting for the model's coarse resolution and the
prescribed dust opacities, it seems plausible that subsurface temperatures on the Gale Crater floor would inter-
mittently reach freezing during Northern Hemisphere Summer and Autumn.

It has to be noted that the large sporadic spikes of methane detected with TLS‐SAM (Webster et al., 2021) cannot
be explained by the seasonal instability of soil seals in the Gale crater. Gale crater is not a unique crater at the low
latitudes on Mars; thus, the abrupt large releases of methane should also happen at other craters. Without an
extremely efficient unknown methane destruction mechanism, the released methane would have been detected by
TGO, which scans all of the Martian atmosphere. The possibility that MSL just happened to land near the only
active methane source on Mars is infinitesimal (Luo et al., 2021; Viudez‐Moreiras et al., 2021). However, the
Gale crater is unique because it is one of only two craters on Mars where a
massive rover drives and drills the surface rocks. We propose a hypothesis for
future studies that the motion of the rover itself or the drilling can cause the
disturbance of the shallow subsurface soil seals and release methane. The
heavy rover can crack a 2 cm soil seal, and Curiosity drills down to 5 cm. If
our hypothesis is correct, then it might be able to explain the abruptness and
seasonality of methane release while the release would remain local to Gale.
To test this hypothesis, it would be beneficial to take methane measurements
when the rover just arrives at a location with abundant high‐salt content
features (like salt veins). Another test would be to try to ingest Martian air
while drilling into the salt‐rich surface.

4.3. Broader Applications of Soil Seals to Astrobiology on Mars

Figure 9. MarsWRF subsurface soil temperatures at 0.5 cm (solid line) and
2 cm (dashed line) depths. The average daily soil temperature (top) is plotted
in addition to the maximum daily temperature (bottom) over the year.
Even though this paper primarily focuses on the potential role of perchlorate
salty soil seals in the variability of atmospheric methane on Mars, soil seals
can have broader applications in astrobiology. Soil seal traps can be potential
habitat locations for Martian microbial life in the shallow subsurface. One of
the severe restrictions on active microbial growth is the low atmospheric
pressure, as demonstrated by Nicholson and Schuerger (2005). Subsequent
studies (Schuerger & Nicholson, 2016) show that some terrestrial microor-
ganisms can grow at pressures as low as 0.7 mbars. However, all experiments

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Acknowledgments
A. P. was supported by NASA's Planetary
Science Division Research Program
through the SEEC ISFM work package at
NASA Goddard Space Flight Center.
Financial support from the NASA Early
Opportunities Program for
Underrepresented Minorities in Earth and
Space Sciences, MUREP Other
Opportunities Program (NASA Award#
NNX16AC90A) is gratefully
acknowledged. S.G. is supported by the
MSL Participating Scientist program. A.P.
is supported as a SAM‐MSL science team
member.
PAVLOV ET AL.
10.1029/2023JE007841
on low‐pressure bacterial growth required continuously hydrated nutrient‐rich media. On Mars, exposure of
hydrated surface soil to low atmospheric pressures would inevitably result in rapid soil desiccation. Any potential
microorganisms in the soil would be desiccated as well. Following our experiments, the overall gaseous pressure
and the water vapor in the soil below the soil seal can be significantly higher than in the atmosphere. Therefore,
below the soil seal, Martian microorganisms would be protected from extreme desiccation and might be actively
metabolizing. Another benefit of soil seals is that they can block UV (Cockell & Raven, 2004) and atmospheric
oxidants (Bullock et al., 1994) from penetrating below the seal. These factors can potentially contribute to the
habitability of the shallow subsurface environment under the soil seals. On Earth, surface mineral crusts exist in
different varieties and require water for their formation, entrap organic molecules, and harbor microbial life.
Biosignatures of surface mineral crusts can be extracted and assayed similarly to search for evidence of life on
Mars (Brolly et al., 2018).
Salt domes found in the Gulf of Mexico basin show extensive carbonate deposits that are formed as cap rock on
top of salt structures (Caesar et al., 2019). These authors have shown that microbial anaerobic oxidation of
methane contributes to carbonate formation in the presence of sulfates. In another recent study (Bayles
et al., 2020), the authors point out that in the Bonneville Basin in the western U.S., similar to what may have
happened on Mars, evaporation of the freshwater lake has left behind huge amounts of evaporite mineral deposits
with high salt concentration where the haloarchaea survive. Such microorganisms may be able to survive the
harsh extreme environment on Mars, especially if they are preserved under the salty soil seals throughout Mars
history.
5. Conclusion
Gas impermeable seals can form in Mars‐like conditions, but they require elevated perchlorate salt content (5%–
10% salts by mass) in the soil and a shallow permafrost layer. The soil seals are several centimeters thick and gas‐
impermeable. Pure ice and salt‐free permafrost do not produce gas impermeable barriers for gases such as
methane. Substantial amounts of gaseous methane (∼3 mbars of pressure differential) could accumulate under the
seal in the shallow subsurface of Mars and be released abruptly into the atmosphere when the seal breaks due to
possibly rover movements, drilling, or impacts. Based on modeled subsurface temperature constraints, soil seals
should be stable over most of the Martian surface indefinitely in the current climate. Gale crater is at the boundary
of soil seal stability, and if present, soil seals can be more susceptible to breaking during late NH Summer and
Autumn. Soil seals provide UV protection, impede water loss, and allow the buildup of gas pressure in the soil
above the triple point of water. Thus, they can provide a habitat for hypothetical Martian microorganisms.
Conflict of Interest
The authors declare no conflicts of interest relevant to this study.
Data Availability Statement
Data for plots are available at Pavlov (2023) and Guzewich (2023).
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