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IN SITU INSTRUMENT OPPORTUNITIES Michael Hecht Jet Propulsion Laboratory, Caltech March 29, 2011 1

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Page 1: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

IN SITU INSTRUMENT

OPPORTUNITIESMichael Hecht

Jet Propulsion Laboratory, Caltech

March 29, 2011

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Page 2: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

What is an “in situ instrument”?

• I prefer the more utilitarian distinction between

planetary surface instruments and orbital or deep

space instruments

• Sensor suggests a transducer, while instrument is a

means to perform an experiment, including sample

handling.

• In addition to chemistry (inorganic and organic),

biology, mineralogy, also have physical properties

(size, shape, density, hardness, thermal

conductivity, etc.) and atmospheric sciences

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Page 3: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

What is in the roadmap: Table 1 (SIOSS challenges)

• Instruments

– Integrated/miniaturized sensor suites

• Sampling

– Subsurface sampling to >1m, cores to 10 cm

– Preservation of sample biological and chemical integrity

– Temperature control of frozen samples

– Unconsolidated material handling in microgravity

• Long term

– Nothing 2017-2022

– Extreme environment technologies (vacuum, microgravity,

radioactive, high/low temperature, high pressure, caustic…

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Page 4: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

What is in the roadmap: Table 5 (Planetary Science needs)

• Mini spectrometer, filters, coatings

• Pulsed lasers (Raman, LIBS) and tunable CW (NIR/IR)

• Gas and elemental composition, APXS, IR, gamma,

Raman, XRD, neutron…

• Geochronology

• Biological sensing

• Sample handling

• High power, extreme environments

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Page 5: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

What is in the roadmap: Table 8 (Sensor technology)

• Particles, fields, waves

• Sample Handling

– Acquisition (subsurface and cores)

– Transfer and delivery

– Cryogenic & sealing (preserve volatiles, control and monitor cross-

contamination

• Chemistry and Mineralogy (beyond APXS)

– Wet chemistry (measure dry weight, dissolved ions to ppm)

– Elemental composition (LIBS, XRF) with spatial resolution

– Mineralogy (Raman, XRD, IR/UV ) with spatial resolution

– Microscopy (SEM, hyperspectral)

• Organics and biology

– Ppb detection (requires contamination control)

– Mass range and resolution (<0.1 amu!)

– Biomarker detection

• Planetary protection

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Page 6: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

QUESTIONS TO PANELISTS

In-situ surface physical, chemical, & biological sensors

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Page 7: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Top sensor challenges (not in roadmap are yellow)

• Imaging with chemical identification, microscopic to

macroscopic

• In situ geochronology

• In situ biomarker detection

• Ultra-high resolution mass spectroscopy (resolve

isobars)

• Lower degree of difficulty:

– Atmospheric instruments

– Physical property instruments

– Geophysics (seismometry, heat flow)

– Terrestrial in situ instruments

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Page 8: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Top system challenges (not in roadmap are yellow)

• MSR curation (in situ)

– Need to avoid alteration as well as loss of volatiles and

cross-contamination. Requires thermal control

• Excavation technologies (rock, soil, ice)

• Extreme environments (Venus, Titan)

• Power technologies

– kW and mW power sources

– Non-solar, non-nuclear (e.g. wind, thermal, chemical)

• Planetary Protection and Contamination Control

– Full-spacecraft sterilization

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Page 9: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

High Priority Sensor Technology Areas (non-biological)

• Liquid phase analysis

– Wet chemistry

– Lab-on-a-chip

– Ice/water analysis

• Mass spectroscopy

– Isobar-resolving (>100K resolving power)

– Laser ablation mass spectroscopy

– Geochronology

• Chemical microscopy

– SEM/EDX

– Small spot scanning XRF

– Spectroscopic imaging

– Chromophor microscopy

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Page 10: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Lower priority sensor technology areas (non-biological)

• Sounding

– Lidar and scanning lidar

– LIBS and Raman

– Neutrons and gammas

– Acoustics

– Seismometry

– GPR

– NMR

– Remote thermal properties

• Other

– Physical properties

– Atmospheres

– XRD

– Electric and magnetic fields

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Page 11: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Alignment with NASA capabilities, role, competitiveness

• All sensor and system technologies listed above

could be well addressed by NASA with appropriate

levels of R&A funding, except possibly:

– Extreme environment operation (large investment,

opportunity for cost-sharing)

– Full-spacecraft sterilization

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Page 12: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Game changing technologies (near tipping point is yellow)

• Ability to do things relegated to sample return, e.g.

– In situ geochronology

– Advanced life detection

– Micro-analysis

• Non-nuclear power sources (e.g. thermal, chemical)

• Extreme environment operation (esp. Venus)

• New architectures:

– Extreme surface mobility

– Broadened access to deep space (flying instruments)

– Ability to collect and store massive amounts of data and

samples with high autonomy, uploading “apps” for data

mining and analysis.

– Fleets of miniature payloads12

Page 13: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

For discussion

• Time horizons for insertion

• Payoffs, risk, technical barriers and chance of

success

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Page 14: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

CHEMICAL MICROSCOPY

Example:

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Page 15: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Big Questions

1. What is the relationship between the airborne dust,

surface soil, and the present-day rock mineralogy, on

Mars in general and at particular sites?

2. What weathering and alteration processes are occurring

presently? What is the contribution of aqueously altered

material to the soil?

3. What does the microstructure of soil tell us about the

spatial extent and time scale of water activity?

4. How local or global is the material observed in the

regolith? What is the spatial distribution? What is the

capacity for transportation of sediment, and how might

it have changed with time?

5. What are the dynamics of the upper meter or two of

regolith? What is the exposure age of the surface? The

exposure history of the subsurface?

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Page 16: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

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Originally the Mars Environmental Compatibility Assessment for the 2001 Mars Surveyor Lander

30 cm

12 cm

The Microscopy, Electrochemistry, and Conductivity Analyzer (MECA)

Page 17: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

1 mmOptical Microscope mosaic

10 µm

AFM topograph

Page 18: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Suggested Approach to Surface Investigation

• Microanalysis

• Diversity

• Subsurface access

• Sample Return

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kaolinite

ESEM/EDX of Calcium sulfate airborne

particles (Iordanidis et al., Environ

Geochem Health 30, p. 391, 2008)

SEM image Courtesy M. Velbel

Page 19: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Wet chemical microscopy

• Microscope slides

coated with

dehydration-resistant

chromophors

• Blue indicates pH in

the example at right

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0.5 mm

Page 20: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Technology roadmap

• Extend microscopy to ESEM

• Add EDX for compositional microanalysis

• Add electron diffraction for structural analysis

• Perform contextual macro-analysis

– Optical and near-IR (e.g. µ-OMEGA), possibly with stains

– Mineralogy with Raman, Mossbauer, XRD

– Surface chemistry with XPS, AES, SIMS

– Surface texture with BET (done by Viking)

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Page 21: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Technology examples

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CO3

CO2

C-CC-O, C-N

XPS probes near-surface region, including

atmospheric species interacting with the

surface (courtesy P. Grunthaner)

Microimaging with ESEM

already uses Mars-like

pressure for charge control and

sample preservation.

Technology is compact

(diagram from Wikipedia, gun

from FEI website)

Electron

energy

analyzer

(SBIR

funded)

Turbo

pump

Al K

X-ray

source

Page 22: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

SOLUBLE CHEMISTRY

Example:

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Page 23: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

How to do in situ chemistry

• Detection of volatiles

– Examples

• Mass Spectroscopy and calorimetry via pyrolysis (TEGA)

• GC/MS via pyrolysis (Viking MS, SAM)

• GC/MS via humidification (Viking biology, SAM)

– Characteristics

• High energy, often only see dissociated fragments

• Wall and gas phase reactions can be a problem

• Only see volatile species

• Aqueous analysis

– Examples

• Electrochemical sensing (MECA WCL)

• Chromatography, electropheresis, colorimetry, etc. (in development)

– Characteristics

• Very low energy

• Only see solubles

• Can’t associate cations with anions

• Limited species can be seen, but large dynamic range

• Reactions can occur in solution

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Page 24: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

The Wet

Chemistry Lab

(1 of 4)

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K+, Na

+

Mg2+

, Ca2+

, Ba2+

Cl-, Br

-, I-

NO3

-/ClO

4

-

CV, CP

pH, Eh, cond., T

Page 25: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

pH Measurement

9

8

7

6

5

pH

12:30 12:35 12:40 12:45 12:50Sol 34

9

8

7

6

5

pH

12:20 12:22 12:24 12:26 12:28Sol 30

Soil Delivery

Open & CloseDrawer

ReleaseAcid

Page 26: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

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Dissolved ions (after re-calibration)

Page 27: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Sulfate titration

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“Blank” (Note: Cl- leak from BaCl2 observed)

Sample

Page 28: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Research implications of perchlorate-rich soil

• Geochemistry and geology:

– Good: Stable brines allow some chemistry and

fluvial processes

– Bad: Uniform distribution suggests soil has

been dry for a long time

• The search for life:

– Good: Microbes use it for energy

– Bad: It’s a desiccant (drying agent)

– Contra-indicative: On Earth, microbes reduce

perchlorate to chloride

– Bad: Where there is perchlorate, there is likely

chlorate, chlorite, hypochlorite…

– Confounding? Perchlorate combusts organics

in experiments such as Viking, TEGA, SAM.

• Human exploration

– Good? Easily extracted for power or O2

source

– Bad? Modest (reversible) toxic hazard 28

Page 29: IN SITU INSTRUMENT OPPORTUNITIES · •High energy, often only see dissociated fragments •Wall and gas phase reactions can be a problem •Only see volatile species •Aqueous analysis

Implications for instrument and mission development

• In situ instrument strategy: Wet or dry analysis?

– Dry analysis needs heat, burns perchlorate

Invest in Lab-on-a-chip, liquid chromatography, etc.

– Pyrolytic approach burns organics

Invest in alternative organic detection such as Urey

• Sample return strategy

– Long-term curation on surface exposes samples to thermal

cycles that have been shown to cause significant secondary

alteration even without brines, which exacerbate problem

– Brine and oxidant formation could destroy organics and

other biomarkers

Possibly severe constraints on surface curation methods

• ESMD interest as in situ resource, possible hazard

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