NASA Technical Memorandum 4184

Scientific Guidelines for Preservation of Samples Collected From Mars

APRIL 1990

Ht/-_I f NASA Technical Memorandum 4184

Scientific Guidelines for Preservation of Samples Collected From Mars

Edited by James L. Gooding Lyndon B. Johnson Space Center Houston, Texas

National Aeronautics and Space Administration Office of Management Scientific and Technical Information Division 1990

5.

Table of Contents iii Executive Summary Preface iv

List of Tables V

V List of Figures

1. Introduction

1.1. Sample Return As Part of Mars Exploration 1

1.2. The 1974, 1977 and 1979 JSC Reports 1

1.3. Need for Updated Report 2 2 1.4. Scope and Purpose

o Importance of Martian Samples 2.1. Nature and Value of Information Contained in Samples 4 4 2.1.1. Planetary composition

2.1.2. Planetary formation and geologic time scale 6

2.1.3. Climate history 6 7 2.1.4. Biological history

2.2. Relative Merits of Laboratory and In Situ Analyses 8

2.2.1. Lessons from Viking Lander Experiments 9

2.2.2. Clues from "Martian" meteorites 9

, Sample Preservation Issues

3.1. Essential Considerations 10

3.2. Contamination 11 14 3.3. Temperature

3.3.1. Sub-freezing (< 273 K) 15

3.3.2. Cool thawing (273-300 K) 16

3.3.3. Sub-sterilization (300-400 K) 16

3.3.4. Sterilization and decrepitation (> 400 K) 16

3.4. Pressure 19 21 3.5. Ionizing Radiation 23 3.6. Magnetic Fields

3.7. Acceleration and Shock 24 25 3.8 Biology and Planetary Quarantine 25 3.9. Summary 4. Recommendations 27

References 29

-- continued -- ii

Table of Contents (continued)

A1-1 Appendix AI: "Call for input" letter, 1974

A2-1 Appendix A2: List of respondents to 1974 call

A3-1 Appendix A3: Letters and data from respondents, 1974

Appendix B 1: "Call for input" letter, 1987 BI-1

B2-1 Appendix B2: List of respondents to 1987 call

Appendix B3: Letters and data from respondents, 1987-88 B3-1

Appendix B4: Estimated concentrations of oxidants in sediment samples at the Viking Lander sites B4-1 iii

EXECUTIVE SUMMARY

Science goals for collecting and returning Based on detailed review of pertinent scientific Martian samples for analysis on Earth, as an literature, and advice from experts in planetary integral part of Mars exploration, are traceable to sample analysis, recommended upper limits for key the National Academy of Sciences and have been parameters in the environmental control of reiterated by various advisory committees and collected samples are as follows: working groups. The desired sample materials include atmosphere, rocks, sediments, soils, deep • Contamination regolith, and possibly ices. The maximum scientific value of the samples is For each element in a geologic sample, retained when they are preserved in the conditions < 1% of the concentration in the that applied prior to their collection. Any sample Shergotty meteorite. degradation equates to loss of information. Contamination by extraneous elements or For each element or compound in an compounds might preclude measurement of native atmospheric sample, < 1% of the Martian chemical or isotopic compositions. concentration in the Viking Lander Excessive warming would mobilize adsorbed atmospheric analysis. water and initiate irreversible chemical or isotope- exchange reactions. Temperatures substantially • Temperature lower than 273 K are required to arrest interfacial water in fine-grained, porous samples. Heat- < 260 K; unweathered igneous rock sensitive materials, including unidentified oxidants < 230 K; soil, sediment, deep regolith, discovered by the Viking Landers, would or weathered rock decompose if excessively warmed. Hydrate or carbonate minerals might undergo stable-isotopic • Pressure (head-space gas, Mars ambient) re-equilibration, thereby erasing their records of ancient Mars climates. Uncontrolled temperature < i atm; unweathered igneous rock rise would also produce large head-space pressures, < 0.01 atm; soil, sediment, deep regolith, through gas desorption from samples, which would or weathered rock further stimulate undesirable reactions. Deliberate heat sterilization would not affect age-dating of Ionizing Radiation 5 g/cm 2 igneous rocks but would profoundly degrade shielding paleoclimate information in sediments and soils. (should not be much lower or higher) Uncontrolled doses of ionizing radiation might erase or obscure the depth-dependent natural • Magnetic Fields < 5.7 x 10-5 T records of cosmic-ray damage in mineral grains. (1 Earth field) The Martian atmosphere differentially filters solar and galactic cosmic rays and changes in sample Acceleration and Shock < 7 g shielding, relative to natural shielding, might alter (1 g = 9.81 m/sec 2) the climate-dependent records of particle tracks and spallation nuclides. Radiation monitors for the Parametric values recommended for the most samples are highly desirable. sensitive geologic samples should also be adequate Extraneous magnetic fields might erase or to preserve any biogenic compounds or obscure natural remanent magnetism in the exobiological relics. samples, or induce magnetic artifacts, that would Additional research would be needed before complicate or even preclude the search for any of the recommended limits could be relaxed on evidence about Martian magnetic fields. scientific grounds. Especially important is the Acceleration and shock loads expected during temperature and pressure dependence of stable a sample-return mission should not threaten the isotope exchange reactions for low-temperature integrity of rocks but might disintegrate soil clods. minerals containing H20 or CO 2. iv

I PREFACE

Many people both inside and outside of NASA This report represents an updated and revised contributed to successful completion of this report. version of work led by Dr. Larry A. Haskin at the The most essential help was provided by Dr. Johnson Space Center in 1974 and that Douglas P. Blanchard, Dr. C. W. Lagle, Mrs. represented one of the earliest attempts to Yvette Damien, Dr. Robert N. Clayton, Dr. scientifically document the case for collecting and Stanley M. Cisowski, Dr. David W. Collinson, Dr. studying well-preserved samples from the planet Edward S. Gaffney, Dr. Henry J. Moore, Dr. Mars. Those valuable and insightful contributions Robert C. Reedy, Dr. Derek W. G. Sears, Dr. have been included in the present version as copies Timothy D. Swindle, Dr. Mark J. Cintala, Dr. John of letters from the specialists who contributed to H. Jones, and Dr. Christopher P. McKay. the original document. New input from other Nonetheless, any lingering errors remain my specialists is recorded here as additional letters that I received in 1987-88, in response to my responsibility. appeal to the scientific community for help in revising the 1974 report. I bear sole responsibility, however, for decisions and interpretations made during integration of the information base.

James L. Gooding NASA Lyndon B. Johnson Space Center Houston, Texas USA January 29, 1990 V •

List of Tables

2.1 Desirable types of Martian samples and their respective values in Mars exploration 4

2.2 Roles of laboratory and in situ analyses of Martian materials 8

3.1 Preservation hazards for Martian samples 10

3.2. Elemental compositions of the Shergotty meteorite and surface sediments at Chryse Planitia, Mars 12

Near-surface atmospheric compositions on Mars and Earth 13

Estimated contamination from Earth's atmosphere for leakage into a 1000 cm 3 Mars sample container at a rate of 10-9 cm 3 STP/sec for 10 days 13

3.5. Volatile-release temperatures of geologic materials heated 10 K/min under 1-atm dry N 2 17

3.6. Temperatures for which one-hour heat treatment anneals nuclear particle tracks 18

3.7 Characteristics of solar cosmic ray and galactic cosmic ray components 21

4.1. Recommended parametric values for preservation of Martian samples 27

List of Figures

1-1 Development of Mars science goals 3

3-1 Maximum surface skin temperatures predicted for Mars as functions of latitude and season 14

3-2 Typical diurnal temperature variations in the near-surface atmosphere at the Viking Lander i and 2 sites 15

3-3 Sub-surface temperature profiles modelled for Vi/a'ng Lander sites 15

3-4 Potential degradation of Martian samples during warming 15

3-5 Seasonal variation of atmospheric pressure a the Viking landing sites 19

3-6 CO 2 gas adsorption on powdered samples of Mars-analogous geologic materials as a function of temperature 19

3-7 Head-space pressures developed by desorption of gases from Mars-analogous materials inside a fixed volume 20

3-8 Production rates of radiation damage effects in Mars surface materials as a function of shielding 21

-- continued -- v±

List of Figures (continued)

3-9 Relative production rates of track damage and spallation 78Kr at the Mars surface and in the deep regolith 22

3-10 Production rates for tracks and spallation nuclides calculated for a lunar basaltic rock directly exposed to SCRs and GCRs 22

3-11 Acceleration-force milestones for Martian samples 24

3-12 Summary of major concerns regarding preservation of collected Martian samples 26 1

1. INTRODUCTION

1.1. Sample Return As Part of (a) To identify those experiments that Mars Exploration could and should be done on returned Martian samples to characterize their Space science organizations in various inorganic properties, countries have consistently recommended exploration of Mars as a high-priority goal. The (b) To evaluate, insofar as can be done, scientific merits of collecting samples on Mars and the effects of potential biological returning them to Earth for analysis have been sterilization of the sample by heating reviewed and endorsed by the U. S. National prior to its return, Academy of Sciences (COMPLEX, 1977, 1978; SSB, 1988), the National Aeronautics and Space (c) To identify particular analytical Administration (NASA) Advisory Council (SSEC, techniques needing further 1986, 1988), the European Science Foundation improvement in order to make (ESF, 1986), and the European Space Agency optimum use of a returned sample, (Chicarro et al., 1989). In fact, after reviewing all and candidate missions beyond the observer-class core program (SSEC, 1983), the NASA Advisory (d) To identify experiments to be done on Council concluded that simulated Martian samples, with and without sterilization, that better define "A sample return mission to Mars before the limits of information available 2000 is the highest priority for an about the planet from analyses of Augmentation Mission to the terrestn'al returned samples. planets" (SSEC, 1986, p. 18).

Planning for a Mars sample-return mission The report was compiled at JSC based on must include a comprehensive review of the input solicited from selected members of the scientific requirements for selecting and acquiring planetary science community, following a call-for- samples on Mars and for preserving them from the input letter from L. A. Haskin (Appendix A1). A time they are collected until the time they are general outline of the study was prepared by five delivered for analysis to laboratories on Earth. The members of the JSC Solar System Exploration purpose of this report is to update previous reviews Division (which was named the Planetary and of sample-preservation goals in a self-contained Earth Sciences Division in 1974) who sent letters to guide for mission planners. The summary the outside science community requesting advice presented here represents an updated and and opinions. Many scientists responded with expanded version of a similar report that was letters that discussed problems and experimental prepared in 1974. approaches in their respective areas of expertise. The list of contributors to the final report (JSC, 1.2. The 1974, 1977 and 1979 1974), and their actual recommendations, are JSC Reports included in this report as Appendices A2 and A3, respectively. In recognition of the major advances in In an independent but concurrent effort, understanding the Moon that were provided by Professor Elbert A. King (University of Houston) return of the Apollo and Luna samples, scientists at organized researchers in various laboratories in a the Johnson Space Center (JSC) prepared a report broad, reconnaissance study of the effects of in April 1974 that summarized the comparable heating on a common set of Mars-analogous goals and strategies for Earth-based analyses of mineral, rock, and soil samples. Both the letters samples returned from Mars. The stated purposes returned to JSC by interested scientists and the of the report (JSC, 1974) were as follows: results of the experiments organized by ProfessorKingwereincludedasappendicesto the 1.3. Need for Updated Report JSC(1974)reportbutarenotrepeatedhere,except assummarystatementsin appropriatechapters. Although much Of the rationale presented in Afterthedeadlinefor receiptof thelettersat JSC (1974) and Bogard et al. (1979) remains valid, JSC had passed,a committeeof scientists considerable progress has since been made in assembledtowritethereport.Towardthatend,a studies of Mars by remote sensing and in meetingwasheldon March27-28,1974at the laboratory studies of lunar rocks, meteorites, and LunarandPlanetaryInstitute(namedtheLunar interplanetary dust particles. In particular, plans to ScienceInstitutein 1974)nearJSC.Membersof sample Mars must take into aceount the following thecommittee(in alphabeticalorder)andtheir developments: affiliationswereasfollows: (a) New knowledge of the Martian S.O.Agrell,CambridgeUniversity, UK environment, gained from analysis of D. D. Bogard, NASA/JSC Viking data (1976-1987). R. Brett, NASA/JSC S. Chang, NASA/Ames Research Center (b) Possible new knowledge of Martian M. B. Duke, NASA/JSC materials, gained (since 1979) from H. P. Eugster, Johns Hopkins University laboratory studies of shergottite, E. K. Gibson, NASA/JSC nakhlite, and chassignite meteorites L. A. Haskin, NASA/JSC (Committee which might be Martian rocks. Chairman) J. C. Huneke, California Institute of (c) Advances in analytical methodology, Technology instrumentation, and laboratory E. A. King, University of Houston geochemical studies (since 1979) that L. E. Nyquist, NASA/JSC would affect mission designs and W. C. Phinney, NASA/JSC sampling strategies. D. W. Strangway, University of Toronto, Canada This report was intended to achieve those H. P. Taylor, California Institute of updates by integrating new information into the Technology excellent frameworks provided by JSC (1974) and S. R. Taylor, Australian National University, Bogard et al. (1979). Australia P. Toulmin III, U. S. Geological Survey, 1.4. Scope and Purpose Reston, Virginia J. L. Warner, NASA/JSC. The purpose of the present report is to provide R. L. Young, NASA Headquarters. a summary, based on current knowledge, of the scientific requirements for collecting and Subcommittees were formed and given preserving Martian samples for laboratory analysis responsibilities for writing individual portions of on Earth. This report is intended to supplement the report. Summaries of major topics were largely and support, rather than replace or compete with, based on the written correspondence that was contemporaneous reports, commissioned by received. NASA, on science or engineering studies of Mars Although JSC (1974) represented an important sample-return missions. In particular, this report is scientific contribution, it was never widely not meant to replace or compete with reports on distributed and carried no formal publication or high-level goals for Mars exploration that will be catalog number that would permit its easy retrieval issued by science working groups that have been by later researchers. To at least partially correct chartered to support mission-design projects. the latter deficiency, and to update the 1974 Instead, this report provides summaries and information in light of results from the Viking traceabilities of requirements at a level of detail missions to Mars (1976-1977), a revised summary that is beyond the scope of the working-group version of JSC (1974) was prepared (JSC, 1977) activities. and published in amended form by Bogard et al. To accomplish the necessary updates relative (1979). to JSC (1974, 1977) and Bogard et al. (1979), a new poll of the science community was initiated in February1987on the subject of sample-science sample preservation derived for the present report goals for Mars. A "Dear Colleague" call-for-input were adopted by MRSR SWG (1989). letter (Appendix B1) was sent to each of 733 In addition, a scientific workshop on the topic addressees, including planetary scientists with of "Mars Sample Return Science" was convened by interests in Mars, Earth-oriented geoscientists, the Lunar and Planetary Institute in November biologists, and selected scientific administrators 1987. As reflected in the workshop report (Drake (Appendix B2). Each person polled was asked to et al., 1988), emphasis was placed on identifying respond to four specific questions: sample requirements to address specific scientific issues. The workshop results were complementary (1) What aspects of Martian history can to, but not identical with, the JSC poll of 1987 and be uniquely (or best) addressed by there remained a need for a cogent summary of direct analysis of samples returned to detailed sample-preservation requirements. Earth? The body of this report represents integration of the text from JSC (1974) with new text that (2) What types and quantities of samples reflects results of the 1987 poll as well as other are needed to support the analyses information compiled from scientific literature related to (1)? published after 1976. Several data figures were added to illustrate points that were either discussed (3) What degrees of sample degradation without graphic aids or not addressed in JSC can be tolerated without defeating the (1974). In general, the material from JSC (1974) analysis goals? (Specify, if possible, was extensively edited and reorganized during upper limits for temperature, merger with the new material. pressure, radiation, acceleration/ shock, etc.). --- 5ECONOARYr--"- couuuNirrSCIENCE =1197",_ 'IP, WHITE ESEPAPER97,] V'T',I It C' (4) What in situ measurements should be I made on Mars to supplement or [COMPLEX, t . I .... replace information that might be lost from degraded samples? i , I t I [SSEC,NAC 1986] _ .... _-,----IPRE,SERVATIO@ -- UPDATED N I ' I ' I [ I WHITE PAPER I A total of 89 written responses were received, 4/ _v f 3 I (Th;_Re.oct) I I I --.-_--J IWRSR SCIENCE I I . I of which 79 contained useful information / , i, /WORKING CROtJp i._._.. J I I I , I I[ MRSR swc, 1959]_ I.p, RAME.17EIC (Appendix B3), including a few from individuals t__ NAS I k • rvAzoi-$ / [ssB. 1985] J/ GENERAL (PT.X, e(c.) who had also participated in the JSC (1974) writing L T _ClUmZMgNrS I ' project. Ten of the responses (not included here) were from individuals who politely acknowledged i the poll but who declined to provide scientific input Figure 1-1. for various reasons, including lack of time or professed lack of expertise. Development of Mars science goals. Post-Viking Shortly after the 1987 poll was initiated, NASA goals are traceable to the National Academy of

chartered a Science Working Group, chaired by M. Sciences (NAS), through its Committee on Planetary H. Carr, to support a renewed study of the options Exploration (COMPLEX) and Space Science Board

for a class of unmanned Mars Rover/Sample (SSB) and have been reiterated by the Solar System

Return (MRSR) missions. Accordingly, the writing Exploration Committee (SSEC), of the NASA

project organized for this report was redirected to Advisory Council (NAC), and the Science Working support the needs and schedules of the MRSR Group of the Mars Rover/Sample Return (MRSR) Science Working Group. Specifically, definition of Project. This report (updated preservation white high-level science goals was de-emphasized in this paper) is focussed on details of sample preservation

report and concentration was focussed on that have not been addressed by various other

identifying detailed requirements for sample committees and working groups. Preliminary results

preservation. The functional synergism among this of this work, however, were adopted by the MRSR

report-writing project, the MRSR Science Working SWG. Group, and previous studies is summarized in Fig. 1-1. Many of the preliminary parametric values for 4

I 2. IMPORTANCE OF MARTIAN SAMPLES

2.1. Nature and Value of Information The well-established scientific case for Mars Contained in Samples sample return has been elaborately presented elsewhere (COMPLEX, 1978; SSB, 1988; Drake et As recognized by the National Academy of al., 1988; Gooding et al., 1989). Rather than repeat Sciences in the light of Viking results, the principal those detailed arguments, the following sections goals of future exploration of Mars must be to review information sought in Martian samples as it establish the chemical, isotopic, and physical state relates to issues of sample preservation. of Martian material, the major surface-forming processes and their time scales and the past and 2.1.1. Planetary Composition present biological potential of Mars (COMPLEX, 1978; SSB, 1988). Those goals can be best met by Major geochemical differences exist among the direct analysis of carefully selected Martian inner planets, as demonstrated by lunar-sample samples under controlled laboratory conditions. studies and by observed differences in planetary Mars Observer, a Mars-orbiting spacecraft which is bulk densities and moments of inertia. scheduled for launch in 1992, will provide global Accordingly, the chemical characterization of any geochemical and meteorological maps of Mars but returned Martian sample is essential. Refinements was never intended to serve as a substitute for a in analytical techniques, resulting largely from sample-return mission (SSEC, 1983, 1986). lunar studies, have enabled experiments on very The correspondence between sample type and small samples (often < 50 mg). Thus, information content is summarized in Table 2.1 and comprehensive information can be obtained from further explained in following sections. minimal material.

Table 2.1. Desirable types of Martian samples and their respective values in Mars exploration

Sample Type Expected Information Content

Atmosphere Elemental and isotopic compositions of gases expelled from the Martian mantle by planetary outgassing; tests for hypotheses regarding volatile-element inventory of Mars and possibility of ancient, dense atmospheres; solar wind interactions

Rock Petrological variety of Martian crust and mantle; chemical processes that differentiated the planet; evidence for core formation; radiometric ages of local bedrock surfaces; absolute calibration of

crater-count ages of surfaces; shock-implanted, trapped-gas samples of ancient atmosphere

Sediment Composition of loose, fine-grained material derived by chemical and physical weathering of crustal rocks. Windblown sediments blanket large portions of the surface and strongly influence

geochemical mapping from Mars orbit. Water-laid sediments might contain chemical and isotopic information about pre-biotic evolution.

Soil Mineralogical, chemical, and isotopic records of local climate during soil development; records of climate change through time as depth-dependent cosmic radiation damage

Deep regolith Chemical, stable-isotopic, and radiation environment of ancient Mars; sub-surface inventory of water and other volatile compounds; test for contemporaneous biogenic compounds or processes

Ice Chemical and stable-isotopic records of water cycles through Mars history 5

Major elements comprising the bulk products and the thermal and tectonic settings of constituents of the terrestrial planets and their formation. meteorites include Si, AI, Ti, Fe, Mg, Ca, Na, K, Secondary minerals (those formed by processes and P. Important minor and trace elements other than igneous crystallization) may result from include H, C, N, S, CI, transition-group metals (Sc surface-related mineral growth and phase changes through Zn), lanthanide or rare-earth elements (La during the chemical alteration processes that have through Lu), Th, and U. Elemental analyses furnish undoubtedly occurred on the Martian surface the basic set of bulk compositional data that is through time. Another important aspect of the essential to the performance and interpretation of planet's history, the record of any living matter, nearly all other experiments done on Martian might be preserved in fossil assemblages which material. Elemental data also furnish an index of could be encountered during studies of secondary- the extent of differentiation (fractional melting, mineral associations. In interpreting petrologic crystallization and liquid immiscibility) of the data, care would be needed to identify Martian materials relative to primordial solar mineralogical changes resulting from sample system matter. In addition, concentrations and collection or storage during Earth return. distributions of the biogenic elements (H, C, N, O, Mars should provide two sources of rock P, S) are essential data in assessing the biological material: endogenous rocks ranging from igneous history or potential of Mars. to sedimentary, and a small proportion of Geochemical studies would focus not only on impact-produced rocks associated with minor elemental concentrations but also on speciation of amounts of exogenous material of meteoritic elements as compounds. Without question, water origin. The igneous rocks may have a wide range would be the compound most highly sought among of compositions and may occur in states ranging the samples. Information derived from water from slowly cooled to quenched. The igneous contents of samples is needed to test models for rocks should consist predominantly of primary outgassing of the Martian interior and the extent minerals of high temperature origin, namely, and time of volcanic activity. It is also related to olivines, pyroxenes, feldspars, silica minerals, and the processes and extent of weathering of primary possibly amphiboles and micas. Some of the rocks Martian surface materials to their present may have been locally subjected to fumarolic or conditions. The relationship between the water in hydrothermal alteration where secondary minerals a sample and the water content of the Martian such as oxides, sulfides, sulfates, halides, atmosphere contains information on secular hydroxides, clay minerals, and zeolites may have variations and Martian atmospheric composition. developed. Measured water abundances will also play strongly Because Mars has an atmosphere containing in models for past or present Martian biology. both H20 and CO 2, it is likely that hydrates and The most fundamental data needed for carbonates occur among the weathering products at interpreting the gross composition of Mars are the Martian surface. Weathering processes on identities of minerals and rocks and their Mars are likely to be both chemical and geochemical properties. Features that must be mechanical, including redistribution of original described and documented include sizes, shapes, secondary minerals and generation of new and surface features of mineral particles and the secondary minerals. nature of fluid inclusions that might have been In addition to single mineral (or phase) trapped during growth of mineral grains. particles, four types of polyphase particles are Mineralogical and petrological examination of expected: igneous rock fragments, sedimentary Martian samples will be exhaustive studies rock fragments, particles with coatings, and involving every returned grain and fragment. indurated soil clods of many particles. The Primary igneous minerals (those formed by mineral-mineral relations, both of an equilibrium crystallization of magmas or lavas) have obvious and a reaction nature, that are preserved in these relevance to such fundamental problems as the types of particles are the most important types of degree of planetary differentiation and the geologic data for deducing Martian rock-forming processes. history of the Martian surface and interior. Major problems to be addressed include volcanic activity and its depth of origin, sedimentary deposits and their transport mechanisms, and metamorphic 6

2.1.2. Planetary Formation and Additional information on the bulk structure Geologic Time Scale and evolution of Mars could be obtained by analyzing fresh igneous rock samples for evidence Planetary gases, originally trapped in the solid of natural magnetization. Natural remanent materials that accreted to form Mars, may have magnetization would imply core formation on Mars been degassed from the Martian interior through in a manner analogous to that on Earth. volcanism and now reside in the Martian Radiometric ages of different magnetic samples atmosphere. The Earth, Moon, Sun and various could help define the history of Mars' magnetic classes of meteorites all possess characteristic field. elemental and isotopic abundance patterns of the trapped noble gases which reflect differences in the 2.1.3. Climate History volatile components of materials that formed these objects. Measurements of such gases in Martian Evidence for atmospheric evolution and atmosphere samples will give an indication of the climate changes on Mars should be preserved as general type of volatile material incorporated by stable-isotopic signatures of volatile elements in a Mars and will aid in the characterization of volatile variety of weathered Martian materials. species present in the early solar-planetary nebula. Oxygen isotope analyses of coexisting minerals Three-isotope oxygen compositions of from a returned Mars sample should prove very individual samples will define the material pool useful in the following ways: from which Mars was formed. Studies of terrestrial (a) estimating the temperatures of formation samples, lunar samples, and meteorites have shown of the mineral assemblages, and that differences in planetary source materials can (b) determining whether or not the minerals be mapped on diagrams of 170/160 VS. 180/160. in such rocks or in the bulk soil were formed in Although 180/160 ratios can change as a function equilibrium, or whether they represent different of temperature in chemical reactions (Section stages of mineral formation. 2.1.3), the three-isotope signature is immutable Certain minerals are inherently much more with respect to geochemical processes and remains susceptible to 180/160 exchange that are others, a fingerprint of the planet. and analyses of these may allow us to monitor Information about the timing and duration of secondary alteration processes that have affected volcanic and metamorphic activity on Mars must the rocks or soil, such as exchange with H20 or come from the applications to samples of one, or CO 2. This type of isotopic study is essential in preferably all, of the radioactive dating techniques interpreting the origin and history of H20 and involving the decay of a long-lived radioactive CO 2 in the rocl_s and the atmosphere of Mars. parent isotope (P) to a stable daughter product Hydrogen isotope analyses (2H/1H or D/H) of (D). The P/D pairs of isotopes which can be used water vapor and hydrous minerals from Mars, in for radiometric age dating are 235u/Z°Tpb, conjunction with 180/160 analyses, should be very 238U/206pb, 232Th/208pb, 87Rb/87Sr, 147Sm/143Nd, useful for the following reasons: 138La/138Ce and 4°K/4°Ar. Radiometric ages (a) they may enable us to evaluate the would provide constraints on the thermal history of contribution of deep-seated igneous (juvenile?) Mars, including formation, crustal differentiation, H20 to the surface rocks and to the atmosphere. and the cataclysmic bombardment evidenced by the If high-temperature igneous or metamorphic heavily cratered surface, as well as the history of minerals such as micas or amphiboles are indeed volatiles and of the hydrologic cycle. found, comparison with the D/H ratios obtained Absolute ages of lava flows are needed to on analogous samples from Earth will be valuable. calibrate geologic ages derived by interpretation of (b) D/H data can aid in defining the total impact-crater densities on various Martian surface amounts of H20 and hydrogen loss from Mars, as units. Impact-metamorphic ages of rocks ejected well as the degree of isotopic fractionation that has from major craters are needed to establish the accompanied such escape. timing of important surface-modifying events. Such (c) D/H analyses are probably the only way to age-dating of craters might be especially important determine the overall contribution (if any) of for craters that appear to have formed in water- or deuterium-free solar wind hydrogen to the Martian ice-laden ground or that appear to closely pre-date atmosphere or surface. or post-date formation of water-cut channels. 7

(d) They may help define the extent of would be expected of extraterrestrial organisms. formation of cosmic-ray spallation deuterium in Such fractionations can be larger than Martian surface minerals. fractionations produced by inorganic mineral (e) They will be very useful in tracing the reactions if the biological reactions are more hydrologic cycle on Mars and in interpreting the effective at low temperatures. Nonetheless, use of temperatures and the mechanisms involved in stable-isotope ratios as fingerprints of biological hydration of Martian minerals and glasses. processes would require detailed understanding of Given knowledge of the isotopic compositions competing inorganic reaction pathways. of both water and minerals, D/H and 180/160 There is a strong possibility that carbonate ratios can be used to deduce temperatures at which minerals will be found on Mars. Measurement of secondary minerals formed through water-mineral 13C/12C ratios in such carbonates will aid markedly reactions. Accordingly, stable-isotopic analyses of in deciphering their origins. Comparison with soils or weathering rinds on rocks are the most similar data for terrestrial and meteoritic materials promising pathways to deriving average will help in interpreting the entire carbon temperatures of ancient climatic regimes. geochemical cycle on Mars. Isotopic comparison of Variations in atmospheric density through Martian carbonates with terrestrial sedimentary time, another parameter expected to serve as an carbonates, which are strongly influenced by index of climate change, could be sought as biological processes, should be important in the variations in cosmic-ray-produced nuclides in search for isotopic signatures of possible Martian surface samples. Galactic cosmic rays penetrate the biological processes. Martian atmosphere and, through high-energy Because there is no evidence for life on Mars nuclear reactions, produce radioactive species in under current conditions (Section 2.2.1), it seems the atmosphere and in the surface minerals. most appropriate to focus attention on the Among the more scientifically valuable, long-lived environmental conditions that either fostered or radionuclides are 14C, 3H, 1°Be, 22Na, 26A1, 39Ar, pre-empted evolution of life during the earliest 53Mn, and 81Kr. Measurement of specific activities period of Martian history. Accordingly, it is of those radionuclides in surface samples can essential to study samples from localities where characterize the spatial and general nature of the water was present during the first 109 years of cosmic-ray flux at the Martian surface. By Martian history and to compare them with samples comparing the activities of very long-lived nuclides where water might be available on present-day (of the order of a million years) with those with Mars. mean lives of only a few years, major changes in the Electron microscopy would be a major tool in density of the Martian atmosphere might be life-science studies as a means for finding detected. microfossils. In addition, direct cultures and biological assays would involve wet-chemical 2.1.4. Biological History procedures. A major effort would probably involve characterization of the trace quantities of highly Studies of possible Martian biology are reactive compounds that produced false positive expected to emphasize identification and results in the Viking biology experiments (Section geochemical characterization of carbon-bearing 2.2.1). Principal tools would include gas and ion materials. The first-order task will be to establish chromatography, mass spectrometry, a_d nuclear that the carbon compounds are native to Martian magnetic resonance and electron-spin resonance samples and not contaminants added by sampling spectrometry. activity. Next, work will focus on whether the In all cases, searches for biogenic compounds carbon compounds appear to be residues of living or biological relics would be predicated upon organisms or abiotic molecular precursors of life access to samples free of degradation or forms. contamination. Carbon isotope measurements (13C/12C ratios) and sulfur isotope measurements (34S/32S ratios) have the potential for helping decide whether organic compounds are of biological or abiotic origins. Appreciable 13C/12C and 34S/32S fractionations are produced by animal and plant metabolism on Earth and similar fractionations 8

2.2. Relative Merits of Laboratory and In Situ Analyses Table 2.2. Roles of laboratory and in situ analyses of Martian materials The mineral separations, chemical treatments, and instrumental sensitivities required for key Preferred Approach geochronological, chemical and biological Measurement Laboratory In Situ measurements make remotely-operated Objective (Earth) (Mars) instruments impractical and point to Earth-based analyses on returned Martian samples as the best Particle-size distribution X means for meeting the stated objectives (Table (requires sieving or other 2.2). Measurements made in situ should be used to physical separations) supplement rather than replace analyses performed in laboratories on Earth. Particle morphology X In contrast with data collected by remotely (requires evaporative coating operated instruments of limited capabilities, and electron microscopy) samples of Mars would never become obsolete. It has been abundantly demonstrated with meteorites Rock identification X and lunar rocks that planetary samples remain fertile sources of new information that are limited (requires thin sections) only by the sensitivity and power of the analytical Mineral Identification X tools that are applied to them. As analytical (may require serial analyses methods advance with time, new information can by multiple techniques) be harvested repeatedly from a single suite of samples. By modern standards, a kilogram of Trace-element chemistry X sample can literally support hundreds of man-years (requires neutron irradiation, of meaningful research. Lunar rocks and soils, for gamma-ray counting and example, are now being productively studied by a possibly wet chemistry) second generation of scientists using analytical methods and interpretational models that were Radiometric age dating X unavailable and, in some cases, unanticipated in (requires mineral separations, 1969 when the first lunar samples were collected wet-chemical processing and (LAPST, 1985). Prospects for study of Martian ultrasensitive mass spectrometry) samples are even greater because it is already clear that Mars is much more complex than either the Stable-isotopic analysis X Moon or the (presumed) asteroid parent bodies of (requires extensive sample most meteorites. pre-treatment and In addition, laboratory analyses of samples ultrasensitive mass spectrometry) permit the greatest possible flexibility in responding to unanticipated properties. Unlike automated Abundance and composition X instruments of fixed design, laboratory analyses can of adsorbed gas use preliminary results to guide the re-design of (gases may desorb experiments in order to achieve analyses of the before Earth return) highest possible precision and accuracy. Automated experiments performed in situ Water content X serve best to analyze those properties that either of regolit h exceed the scale of a returnable sample or that are (metastable ice may evaporate; unlikely to survive during return of the sample to level of heterogeneity may Earth. Because of the latter consideration, sample exceed sample size) preservation and in situ experimentation should be orchestrated in roles of mutual support. Practical limitations of sample preservation should exert a strong influence on selection and design of experiments to be performed on Mars. 9

2.2.1. Lessons from _king Lander 2.2.2. Clues from "Martian n Meteorites Experiments If shergottite, nakhlite, and chassignite (SNC) Material properties of the Martian surface at meteorites are rocks delivered to Earth by the two Viking landing sites were summarized by meteoroid impacts on Mars (e.g., Wood and Arvidson et al. (1989). Results from Lander 1 Ashwal, 1981), why then do we need additional (Chryse Planitia, 22.482 ° N, 47.968 ° W) were samples? The answers fall into two major generally consistent with those from Lander 2 categories. First, in the absence of independently (Utopia Planitia, 47.996 ° N, 225.736 ° W) . The documented samples from Mars, it is logically Landers made no mineralogical analyses but impossible to establish with certainty that the SNC performed several experiments that revealed some meteorites are Martian rocks. Only one of the of the chemical properties of sediments and soils eight meteorites in question, namely the Elephant within about 25 cm of the surface at Lander 1 and Moraine, Antarctica, A79001 shergottite within about 6 cm of the surface at Lander 2. No (EETA79001), contains physical evidence that links rocks were analyzed at either site. it directly with Mars. Glassy inclusions in All three biology experiments produced EETA79001 contain trapped gases that resemble positive results for active surface chemistry among the Martian atmosphere (as analyzed by Viking fine-grained materials at both landing sites but Landers) both in elemental and isotopic absence of detectable organic compounds composition (Bogard and Johnson, 1983; Becker (apparently less than a few parts per billion) argued and Pepin, 1984) as well as relict grains rich in strongly against life-based processes as the correct sulfur and chlorine that compositionally resemble explanation (Klein, 1978). It is now clear that the sediments at the Viking landing sites (Gooding designing remotely operated experiments that will and Muenow, 1986). give unambiguous answers to critical life-science Second, even if SNC meteorites are genuine questions is exceedingly difficult, if not impossible. Martian rocks, they were randomly selected and by Consequently, the prevailing body of scientific no means represent the suite of samples that is thought now endorses detailed Earth-based studies needed to answer first-order questions about Mars. of returned samples as the only effective means of For example, the SNC meteorites are all igneous assessing the biological prospects for Mars rocks from unknown geologic terranes so that their (COMPLEX, 1977). radiometric ages provide few constraints on ages of The Viking results did reveal the presence in surface-forming units on Mars. Furthermore, they the near-surface sediments of chemical species that carry little, if any, information about the can fix carbon from gaseous CO 2 and that oxidize mineralogy and volatile-element inventory of organic compounds such as Na-formate (Klein, Martian soils and sediments or evidence about 1978). In addition, at least one of the unidentified climate changes. Nonetheless, discovery of species evolves gaseous 0 2 by reaction with water. carbonate minerals (Gooding et al., 1988) and The reactive species occur at the parts-per-million associated traces of possible organic matter level of concentration (Appendix B4) and can be (Wright et al., 1989) in shergottite EETA79001 deactivated (presumably decomposed) by heat argues strongly for existence of materials that treatment. In addition, the t'me-grained sediments would require careful preservation. contain significant quantities of adsorbed The strategies and methodologies appropriate atmospheric gases (Oyama and Berdahl, 1977) and for analyzing returned Martian samples can be approximately 1-3% water by weight (Biemann et illustrated by reference to work performed on SNC al., 1977; Anderson and Tice, 1979). meteorites. For example, an intensive consortium The bulk elemental compositions of surface study of the Shergotty, India meteorite, the type sediments, which are probably highly oxidized, are specimen for shergottites, was performed on less rich in Fe, S, and CI (Clark et al., 1982) and contain than 25 g of material but produced data on trace- approximately 1-7% of a strongly magnetic mineral element compositions, radiometric ages, (Hargraves et al., 1977). The bulk-elemental cosmogenic nuclide abundances, noble-gas compositions and biology results have been used to abundances, stable-isotopic compositions, and argue for a sediment composition dominated by general petrology (Laul, 1986 and papers in same smectite clay minerals (Banin and Margulies, 1983) issue). -- materials that would require special handling during collection and Earth return. 10

3. SAMPLE PRESERVATION ISSUES

3.1. Essential Considerations and IM is the difference in information content between pristine and returned samples that must The value of analyses to be made on returned be recovered through in situ analyses on Mars. Martian samples could be seriously weakened if the Ideally, each sample collected on Mars would samples are not properly preserved from the time be returned to Earth under conditions that were they are collected until the time they are received identical to those of the environment from which it in laboratories on Earth. In essence, sample was collected so that IR]Is = 1. Complete fidelity degradation equates to loss of information. of preservation would assure that sample Although susceptibility to degradation can be properties measured on Earth were truly expected to vary as a function of sample type and representative of the natural environments on measurement category, the parameters that are at Mars. No single set of preservation conditions the heart of the sample-preservation issue are can be specified, though, because no single set of defined in Table 3.1. environmental conditions applies to all places on The information equation pertaining to Mars. Mars is a dynamic planet with temperatures material analyses of Martian samples is and atmospheric pressures that vary with latitude, longitude, and elevation, as well as with season. In Is = IR + IM [3-1] addition, at any one landing site, samples collected from depth will have experienced different where the Is denotes information contained in temperatures, pressures, and radiation environments than those at the immediate surface. pristine (unaltered) samples on Mars, IR represents information retained in samples returned to Earth,

Table 3.1. Preservation hazards for Martian samples

Hazard Definition

Contamination Addition of extraneous solid, liquid, or gaseous matter that would complicate,

compromise, or preclude measurement of natural chemical or isotopic compositions of

a sample

Temperature Increase of temperature that would foster decrepitation of solids, evaporation or

desorption of volatile elements or compounds, or chemical or isotope-exchange

reactions among components in a sample

Pressure Increase or decrease in confining (head space) gas pressure that would lead to

desorption or surface displacement of volatile elements or compounds,

or solid-gas reactions

Ionizing Radiation Bombardment of a sample by protons, neutrons, alpha or beta particles, or photons

(including X-rays or gamma rays) that would produce radiation damage or

obscure the record of natural radiation on Mars

Magnetic Fields Exposure to magnetic lines of force that would obscure natural remanent magnetism

in a sample or introduce remanent artifacts

Acceleration and Shock Mechanical disturbances that would alter or obscure natural physical attributes of

a sample, including porosity, grain shapes, particle-size distributions, degree of

induration, or layered sequences 11

Exact duplication of Martian conditions after 3.2. Contamination sample collection may be either impossible or impractical for various reasons. Accordingly, the The chemical, mineralogical, isotopic, and problem of sample preservation is best approached biological properties of Martian samples are sought by identifying the probable scale of information as keys to the similarities and differences between loss from samples as a function of the deviations of Mars and Earth. Accordingly, Earth materials preservation conditions from natural Martian must not be allowed to contaminate the Martian conditions. In essence, the objective is to samples in ways that would confuse or mislead understand how the IR/IS ratio changes with research efforts. In addition, steps should be taken collection and preservation conditions. Preferred to minimize cross contamination among different conditions for preservation will be those that yield Martian samples so that natural variations will not IR/Is ratios close to unity. be obscured. Threats to the pristine conditions of samples The ultrasensitive analytical methods to be fall into two categories: applied to Martian samples will seek precise determination of elemental concentrations and • Incidental degradation during collection and variations among elemental and isotopic ratios. return Samples will be sub-divided into their component parts and analyzed as the smallest practical • Deliberate degradation by sterilization. aliquots. Consequently, even minute quantities of extraneous contaminants could have profound Incidental degradation covers all types of effects on the measured properties. alteration caused by sampling or mission Table 3.2 gives the minimum set of elements operations whereas deliberate alteration would be that will be analyzed in Martian samples. attributable to pre-plarmed, precautionary Regardless of whether shergottite meteorites are biological sterilization of samples. Martian rocks (Chapter 2), the data in Table 3.2 Acquisition of samples on Mars would pose illustrate the order-of-magnitude concentrations risks principally in the areas of material expected for various elements in Martian geologic contamination and thermal degradation. Debris samples. Contamination would occur if extraneous abraded or shed from sampling tools, containers, or matter introduced an element into a sample at a other items of hardware must be minimized and concentration that approached or exceeded the restricted to innocuous materials. Likewise, natural concentration of that element in the mechanical energy transferred from tools to pristine sample. Clearly, Martian samples will be samples during collection operations must be extremely sensitive to contamination for elements regulated to prevent excessive heating of the that occur naturally at the parts-per-million or samples. parts-per-billion levels. In contrast, a few ppm The conscious decision to biologically sterilize contamination by iron or aluminum would be more returned Martian samples to preclude tolerable because Fe and AI occur naturally at contamination of Earth by alien life forms would concentrations of several weight percent. profoundly affect the design of the sample-return For example, indium-silver metal alloy was mission. Biological sterilization of materials is employed as a seal material in boxes used to normally accomplished by heat treatment, chemical containerize lunar samples on the Moon (Allton, treatment, or application of lethal doses of ionizing 1989). Unfortunately, later attempts to measure radiation. All three methods would be offensive in the intrinsic concentrations of volatile siderophile different ways to one or more categories of elements (at ppb concentrations) in some of the analyses that would be planned for returned lunar samples fell into question because of possible Martian samples. In contamination. The following sections discuss in detail each of Curation of Martian samples on Earth will the issues called out in Table 3.1. For probably utilize procedures for non-contamination documentation, reference is made to published that were developed for lunar samples and literature as well as to letters received from meteorites. However, those efforts can never individual scientists and provided in Appendices A3 reverse contamination introduced during sample and B3. Summaries and recommendations are collection and packaging on Mars. Therefore, provided in Chapter 4. procedures used on Mars should be designed for minimal contamination of the samples. 12

Table 3.2. Elemental compositions of the Shergotty Table 3.2. (continued) meteorite and surface sediments at Chtyse Atomic Planitia, Mars (Viking Lander 1) in percent (%), No. Shergotty a Marsb parts per million (ppm), and parts per billion (ppb) by weight 56 Ba 27-40 ppm 57 La 130-2.44 ppm Atomic 58 Ce 3.51-6.4 ppm No. Shergotty a Mars b 59 Pr 0.70-0.88 ppm

2 He 0.19-0.21 ppb c 60 Nd 2.60-4.7 ppm

3 Li 3.3-5.6 ppm 62 Sm 1.01-1.89 ppm 6 C 430-620 ppm; 44-210 ppm d 63 Eu 0.43-0.65 ppm 7 N 132-794 ppb e 64 Gd 1.64-2.8 ppm 8 O (40.7-43.6%) h 65 "It) 0.41-0.52 ppm

9 F 41-42 ppm 66 Dy 2.16-4.8 ppm 10 Ne 0.015--0.017 ppb c 67 Ho 0.56-0.86 ppm 11 Na 0.95-1.09 % 69 Tm 0.30-0.38 ppm

12 Mg 5.40-5.7 % 3.6 % 70 Yb 1.19-1.80 ppm 13 AI 3.60-4.02 % 3.9 % 71 Lu 0.18-0.26 ppm 14 Si 23.1-24.0 % 21% 72 i If 130-2.23 ppm 15 P 0.24-0.35 % 73 Ta 0.18-0.29 ppm 16 S 0.13-0.16 % 2.7 % 74 W 0.4-0.5 ppm

17 C1 108 ppm 0.8 % 77 lr < 5 ppb 18 Par 3.3-9.9 ppb c 79 Au 0.81-16 ppb 19 K 0.12-0.16 % < 0.4% 81 TI 0.15-14.0 ppb 20 Ca 6.80-7.15 % 4.1% 82 Pb 94 ppb f

21 Sc 52-59 ppm 83 Bi 0.47-2.4 ppb 22 Ti 0.4-0.5 % 0.37 % 90 Th 0.25-0.39 ppm

23 V 260.-265 ppm 92 U 0.055-0.17 ppm 24 Cr 0.12-0.16 % a Laul et al. (1986), except where noted 25 Mn 0.40--0.42 % b average "deep" sample; Clark et al. (1982) 26 Fe 15.1-15.6 % 12.2 % c all isotopes; Becker and Pepin (1986) 27 Co 37.2-45 ppm d excluding C extracted at < 600 C; Wright et al. (1986) 9_8 Ni 56-88 ppm e excluding gas extracted at < 600 C; Becker and Pepin (1986) 29 Cu 26-54 ppm f sample 3A; Chen and Wasserburg (1986) 30 Zn 62-83 ppm g Clark et al. (1976) 31 Ga 15-17.6 ppm h by difference from sum of major elements 33 As 0.025 ppm

34 Se 0.29-0.47 ppm Apollo designs were required to avoid Pb, U, 35 Br 0.60-0.89 ppm Th, Li, Be, B, K, Rb, Sr, noble gases (He, Ne, Ar, < 30 ppmg 37 Rb 4.5-7.27 ppm Kr, Xe), rare earths (La-Lu), microorganisms, and 38 Sr 45-51 ppm 60 ppmg organic compounds; those same contaminants 39 Y - 70 ppmg (including In and other trace siderophile elements) < 30 ppmg 40 Zr 50-67 ppm should be avoided among Mars sample tools and 42 Mo 0.37 ppm containers. Acceptable Apollo materials included 47 Ag 6.8-110 ppb Teflon, aluminum, and certain stainless steel alloys 48 Cd 0.014--0.34 ppm (Allton, 1989). Mars tools and containers should 49 In 0.023-0.026 ppm be fabricated of materials that are chemically 51 Sb < 5 to 20 ppb nonreactive and that can be readily recognized as 52 Te 3.2-19 ppb artificial if unavoidably introduced into a sample. 53 I 0.036-0.050 ppm Ideally, each tool/container material should be 55 Cs 0.36-0.48 ppm homogeneous and possess distinctive chemical and isotopic signatures that would permit its reliable - continued - "subtraction" from an analytical data set. 13

Forgeologicsamples,contaminationbyagiven (Table 3.2) suggest salt minerals that might be rare chemicalelementshouldbetolerableif it doesnot or absent in the rocks. The oxidation states and exceeda smallfractionof theconcentrationof the mineralogical compositions of rocks and elementaslistedin Table3.2. Forexample,the soils/sediments are also expected to differ Fi/a'ngLandersfoundno fLxedcarbonin near- significantly. Furthermore, if SNC meteorites are surfaceMartiansedimentsatthedetectionlimitsof Martian rocks (Chapter 2), then at least three a few ppm. Exceptfor tracesof carbonate different rock types exist on Mars. In any case, minerals,thetotalcarboncontentsof shergottite neglect of cross-contamination issues could meteoritesareonlya fewhundredppm,mostof unnecessarily complicate laboratory analyses of the whichmightrepresentterrestrialcontamination. samples and, in the worst case, prevent recognition In fact,if thecarbonextractedfromthesamplesat of subtle differences among samples. < 873 K is dismissedas contamination,the Little or nothing can be done about concentrationsof indigenous,non-carbonate contamination of rocks by fine-grained soils or carbonin shergottitesmightbe aslowas44ppm sediments with which they are naturally associated. (Wrightet al.,1986). Accordingly,anycarbon It is more important that care be taken not to mix contaminationof Martian samplesshouldbe different types of rocks or different types of assiduouslyavoidedandlimitedto < < 44 ppm. soils/sediments. Given the apparently high oxidizing potential of Martian soils (Section 2.2.1; Appendix B4), a property not displayed by lunar soils, the materials- Table3.3. Near-surface atmospheric compositions (volume compatibility problem will require further study. basis) on Mars (Owen et al., 1977) and Earth. Materials that might be stable with respect to

reaction under lunar conditions might exhibit Mars Earth corrosion under Martian conditions. CO2 95.3 % 0.03 % Because the Martian atmosphere is only about 1% as dense as Earth's atmosphere and very N2 2.7 % 78.1% different in elemental composition (Table 3.3), Ar 1.6 % 0.93 % atmospheric samples collected at Martian ambient 02 0.13 % 21.0 % pressure could be highly susceptible to CO 0.07 % < 1 ppm contamination. Any off-gassing by spacecraft systems or any subsequent leakage of Earth H20 0.03 a % 0.8 b % atmosphere into the sample containers would 03 0.03 ppm < 0.1 ppm seriously degrade the samples. Container leak Ne 2.5 ppm 1800 ppm rates estimated by Bogard et ai. (1979) are summarized in Table 3.4. For the conditions Kr 0.3 ppm 100 ppm postulated, it was found that a Mars atmospheric Xe 0.08 ppm 8 ppm sample at Mars-ambient pressure could become a Typical value; known to vary contaminated with Earth atmosphere at the level of b 50% relative humidity at 298 K 0.1% within 10 days for most gases except CO 2. Because CO 2 occurs at such a low concentration in Earth's atmosphere, the partial pressure of CO 2 would be greater inside the Mars sample container Table 3.4. Estimated contamination from Earth's atmosphere than outside it. Consequently, there would be only for leakage into a 10C0 cm 3 Mars sample container minor contamination by inward diffusion of CO 2. at a rate of 10 -9 cm 3 STP/sec for 10 days (Bogard For all other gases, however, partial pressures ¢t al., 1979). inside would be less than those outside and the net CO2 Negligible tendency for inward leakage of gas would represent a significant contamination threat. N2 7 x 10 -4 cm 3 STP Cross-contamination between samples should Ar 9x10 "6 also be minimized. Although the compositional 02 2 x 10 -4 variations across the Martian surface remain to be Ne 2 x 10 -8 determined, at least two fundamentally different types of samples can be postulated. High sulfur Xe 8 x 10 -11 and chlorine concentrations in the soils/sediments 14

3.3. Temperature a given sampling locality on Mars, the appropriate preservation temperature for a sample taken from Possible effects of temperature rise on Martian depth will generally be tens of degrees lower than material can be separated into two categories: for a sample taken from the free surface. decrepitation and reaction. Decrepitation occurs Samples from areas poleward of 80 ° latitude when solid phases containing volatile elements would be accustomed to < 200 K at all depths (Fig. decompose with evolution of gas. In the broad 3-1). Accordingly, it is samples taken from polar sense, decrepitation can also include irreversible areas or from depth at any latitude that could be desorption of gases from solid surfaces. Chemical most sensitive to uncontrolled temperature rise. reactions involve destruction of original phases and Many different changes in Martian samples possible creation of new phases whereas isotope- can be expected as temperatures rise from Mars exchange reactions involve redistribution of isotopes ambient values (Fig. 3-4). Although the melting of a given element among various chemical phases. point for water ice (273 K) is a well-known Temperatures at the upper skin of the Martian milestone, processes unfavorable to sample surface vary greatly with both latitude and season preservation can also occur at sub-freezing (Fig. 3-1) and with time of day (Fig. 3-2). Below temperatures. Above the melting point, major the surface, however, temperature variations are changes are expected and, above the biological increasingly moderated with depth so that, even sterilization interval (about 420-430 K), changes during daytime in summer, samples taken from would be profound. Detailed accounts of the depths greater than 25 cm will be 30-50 K colder possible temperature-related sample degradations than at the upper surface (Fig. 3-3). Therefore, at are given in the following sections.

SPRING SUMMER AUTUMN WINTER EQUINOX SO LSTIC E EQUINOX SO LSTIC E 90 II \%2°° i

60 F 27O I I "_X1270 1260 xL 280_

...... i ...... " ......

--Z30

-60

-90 i 0 90 180 270 360 AEROCENTRIC LONGITUDE (dec])

Figure 3-1.

Maximum surface skin temperatures (degrees Kelvin) predicted for Mars as functions of latitude and season (modified

from Kieffer et al., 1977). All seasonal milestones refer to the northern hemisphere. Relative to the surface

temperatures shown here, sub-surface temperatures should be colder at all locations (see Fig. 3-3). Also, because of

differential heating effects, the surface skin temperature will tend to be warmer than that of the near-surface atmosphere

at the same location (compare with Fig. 3-2). Viking Landers 1 and 2 sampled latitudes 22 ° N and 48 ° N, respectively,

with the primary missions occurring during northern summer. 15

3.3.1. Sub-Freezing (< 273 K) Heating to 235 K could foster development of Samples heated to 200 K should see any cubic liquid-like capillary water on clay-mineral water ice converted to ordinary (hexagonal) water substrates. Survival of unfrozen water to such low ice, sublimation of any CO 2 ice, and incipient temperatures has been documented for desorption of permanent gases such as N2, 02, and montmorillonite-water systems by numerous Ar. Heating to 230 K would substantially desorb laboratory experiments (e.g., Anderson and gaseous CO 2 (see Section 3.4) and begin Morgenstern, 1973). Even though the capillary liquifaction of any Ca,Mg-chloride brines (Brass, water might not be truly liquid in the strict, 1980). thermodynamic sense, its mobility might be sufficient to foster ionic migration and, therefore, aqueous geochemical processes in the ostensibly frozen sample. Both chemical and isotope- 240 exchange reactions might ensue. ,_ 2_,ol

L,J

WATER- hCE TRANSITIONS 220 //'_L--2,5o, 45 _, Ic m, 12_si 12_oi i 2so i 27_

C02 iCE IW AT [[Q -ICI EVAPORATES GASES MELTS OESOR9 OR,RF_LIQUFEY ! i I,/ CAPILLARY WATER r ._,.._;.._ LIO, JID MDSILIZES " i " ;" lgo; P TEMPERATURE I-[20 ICE/VAPOR _. I IBO t MILESTONES iSOTOPE EXCHANGE 0 4 8 12 16 20 24- FOR MARTIAN SALT--tdlNERAL/WATER P IS 0 T O':_E LOCAL LANDER TIME (fir) 5A MPLES EXCHANGE BIOCHEMICAL _ COMPOUNDS DEGRADE p Figure 3-2. Vl.ljE SUMMER ATM. CARBONATE TRANSITIONS _o

MARS SUMMJCR SUflI',ICE _'4 ¢11 plrPI'H :

Typical diurnal temperature variations in the near- wsvLzrde,v_.(z_wj: - _ ! . !i . -',I

surface atmosphere at the Viking Lander 1 and 2 120 140 1,60 180 200 220 240 260 280 301 TEMPERATURE [K) sites (modified from Hess et al., 1977). Local noon

is at 12 hr and midnight is at 0 and 24 hr. ERATURE MILESTONES FOR MARTIAN SAMPLES ]

I* CLAY-MINERAL H20(+} LOST P " /,/.Fe-0XYHYI)ROXIDE H20{+} LOST ] MAOHEMITE/HEMATITE TRANSITION TEMPERATURE (K) • iI " TROILITE/P_RHOTITE TRANSITIONS 1_3 190 200 210 220 230 240 25,0 260 270 0 . . . CLAY-ZE DLITE/WAIER I ISOTOPE EXCHANGE " ZEOLFFES DEHYDRATE

i _ CLAY-MINErAL H,7.0(-) LOST r : V£, OXID,_NT_ DECOMPOSE

SALT-MINERAL H20(÷) LOST / :_ I 22° N " \ //-_VL-Z I--BIOL_ICA_ E_RIUZArloI¢ / duly 24, 1976 _, _,' [ --_" _NESQU[HONITE (Id,II.-.CAI_gIONATC) TRANSITION

i /l/ S.L _, lg76 ]oo 4.00 500 600 700 800 900 I ooc :° i/V TEMPERATURE (K) Figure 3-4. 251

Potential degradation of Martian samples during Figure 3-3. warming. "VL" temperature ranges are those

measured at the Viking Lander sites during northern Sub-surface temperature profiles modelled for summer. The 24-cm temperature corresponds to Viking Lander sites (after Kieffer, 1976). For each Fig. 3-3. Note that liquid-like capillary water can landing site, the two-limbed envelope shows the form at temperatures as low as 235 K and that temperature limits expected during one day-night thermodynamically liquid water can form at > 263 cycle. At depths > 25 cm, though, samples would K. The 423 K "sterilization" milestone is only a have probably experienced temperatures no higher typical temperature within the dry-gas sterilization than about 220 K. range of 390-590 K. 16

irreversibly decompose by reaction with available Heating to 263 K could form true liquid water water to liberate oxygen gas. despite the fact that pure bulk ice exhibits At 280-290 K, any vaterite (a low-temperature equilibrium melting at 273 K. Extensive studies of the physics of soil mixed with geologic materials polymorph of CaCO 3) would irreversibly invert to have shown that incipient melting of ice calcite. Accordingly, possibly important details about carbonate formation on Mars would be disseminated in a f'me-grained, porous medium can occur at tens of degrees Kelvin below the 273 K irretrievably lost. milestone. Above 263 K, this unfrozen water occurs as f'rims that are many molecular layers thick 3.3.3. Sub-Sterilization (300-400 K) (McGaw and Tice, 1976). Therefore, it appears that water-based chemistry could proceed in any Several different processes of irreversible ostensibly frozen soil at temperatures> 263 K. change would begin above 300 K. First, any Professor John Oro (personal communication, hydromagnesite (a hydrous Mg-carbonate) would irreversibly invert to nesquehonite, thereby 1987) suggested that degradation of certain highly sensitive biochemical compounds begins at destroying important details about carbonate formation on Mars. Next, various hydrated temperatures of 253-263 IC Franks (1982) reviewed evidence for measurable reaction rates of minerals, including sulfates, clay minerals, and zeolites, would begin to lose water. Some of the enzymes at temperatures as low as 250 K. water loss would be reversible because later Therefore, concerns for biological materials would humidification could partly or wholly restore the seem to require preservation at sub-freezing lost water. The stable-isotopic composition of the temperatures. Stable-isotope exchange reactions can also original water, however, would be information that could not be reconstructed. proceed at sub-freezing temperatures. Notable As shown by the Viking Lander biology examples include oxygen exchange between calcite and water and deuterium exchange between liquid experiments (Klein, 1978), the trace quantities of oxidants in Martian sediments decline in reactivity water and water vapor (Friedman and O'Neil, upon heating over the 320-400 K range. Available 1977). For salt minerals at sub-freezing evidence suggests that more than one oxidant exists temperatures, oxygen exchange might be sluggish and that the loss of reactivity is irreversible and but hydrogen exchange might be significant over results from decomposition of the oxidants periods of months (Kyser, 1987). Because water-based chemical or isotopic (Appendix B4). Consequently, any hope of changes would comprise some of the most rapid identifying the oxidants in returned Martian and serious sample degradations, preservation samples would be lost if the samples were heated above about 320 K. temperatures must address the issue of unfrozen In this temperature interval, hydrogen and water. For deep Martian samples that might never oxygen isotope exchange reactions, between solids have experienced temperatures > 230 K, relaxation and water vapor or liquid water, would occur of preservation temperature to 273 K might invite a host of undesirable and irreversible chemical and readily for most non-silicate minerals and carbon isotope exchange reactions involving carbonates isotopic changes. would become more rapid (Kyser, 1987). 3.32. Cool Thawing (273-300 K) 3.3.4. Sterilization and Decrepitation

Above 273 K, any ice would be converted to (> 400K) liquid water and both chemical and isotope- Above the temperature generally recognized as exchange reactions would greatly accelerate. Both adequate for biological sterilization (423 K), many hydrogen and oxygen exchange reactions would be profound chemical and mineralogical changes significant on the time scale of months for CO 2- would occur in samples. The treatment given H20 gas systems and for some hydrated salt below will not address biological concerns which, minerals; carbon isotope exchange reactions would be significant for CO2-CO3 z- in aqueous solutions by definition, are abdicated by electing sterilization. Instead, geochemical consequences of sterilization (Kyser, 1987). will be emphasized. The most important The trace oxygen-rich compound(s) discovered mineralogical effects of decrepitation would be loss by the Viking Lander Gas Exchange (GEX) experiments (Oyama and Berdahl, 1977) would of H20 from hydrous silicates, oxides, and salts 17

andloss of CO 2 from carbonates. Devolatilization Table 3.5. Volatile-release temperatures of geologic is most pronounced for heating under vacuum, materials heated 10 K/min under 1-atm dry N2 where volatiles are removed continuously. (adapted from Kotra et al., 1982) Hydrated silicates most susceptible to this type of degradation are clay minerals and zeolites; those

least susceptible are amphiboles and micas. Temperature (K) of Initial Critical temperatures and products of Decrepitation (H20 Ioc_,

sterilization-induced mineral reactions can be Mineral unless otherwise noted) expected to vary with the total pressure and gas composition (especially partial pressure of water Gocthite, FeO(OH) 493-513 vapor, PH20) in contact with the sample. Dry Diaspore, AdO(OH) 673 sterilization (i.e., performed without steam) is Siderite, FeCO3 738 (CO2) normally accomplished by heat soaking at 390-590 Magnesite, MgCO3 703 (CO2) K for a few hours (time varies inversely with Calcite, CaCO 3 933 (CO2) temperature); two hours at 423 K would be typical. Dolomite, CaMg(CO3)2 903 (CO2) Transition temperatures expected under low- FeSO4 • 7 H20 373; 873 (SO2) pressure, dry conditions are those depicted over the Fe2(SO4)3" n H20 373; 873 (SO2) 300-1000 K range in Fig. 3-4. Other details can be MgSO4 • 7 H20 373; 1143 (SO2) found in letters by Hower, Fournier, Anderson, Gypsum, CaSO4 "2 H20 383 Papike, and by Bence, Smith, Baily, Skinner, and Dickite, Ad2Si205(OH)4 673 Sato (Appendix A3). Kaolinite, Ad2Si2Os(OH)4 713 For many different Mars-analogous minerals, MontmoriUonite, 848 Kotra et al. (1982) experimentally verified the (Na,Ca)0.3(Ad,Mg)2Si4010(OH)2 "n H20 expected devolatilization reactions (Table 3.5). Threshold temperatures for devolatilization vary with heating rate, atmospheric pressure, and gas Perhaps the most delicate property to be composition. For a given heating rate, affected by sterilization is the extent of oxidation. devolatilization began at lower temperatures under Determination of the intrinsic oxygen fugacity of vacuum, relative to one-atmosphere experiments. igneous minerals would be extremely important to For a constant heating rate and pressure, define the role of oxygen in Martian volcanic decarbonation began at substantially lower processes and the origin of the Martian temperatures under N 2 than under CO 2. atmosphere. However, as Sato and Wones point Accordingly, decrepitation of carbonates during out in their letters (Appendix A3), the preservation sterilization could be retarded by high pressures of of the oxidation state of the returned sample CO 2 but carbon and oxygen stable-isotopic depends critically on any sterilization. Heating in exchange reactions between the carbonates and the vacuum entails loss of hydrogen and a change in CO 2 might be extensive. oxidation state. If graphite or other carbon-bearing The effects of internal reaction are more material (including carbonate minerals) is present, difficult to access and depend initially on the levels heating may produce chemical reduction of silicates of PH20 reached during sterilization. These levels and oxides. To overcome the loss of hydrogen, the will be highest if heating occurs in a sealed sample could be sealed within a sample chamber container and either water is added or a large lined with ultrahigh-purity gold. amount of hydrous material is originally present in Rates of thermal decrepitation should be the sample. In general, sterilization under high controlled by formation of devolatilized surface PH20 should skew the onset of potential reactions layers which slow the outward diffusion of to lower temperatures and increase their rates. additional volatile compounds through the surface. Feldspars would probably suffer surface alteration Careful, well-conceived experiments are still to mica-like phases whereas olivines, pyroxencs, needed to quantify the kinetics of such processes. and amphiboles would probably develop surface In addition to the mineral decrepitations layers of chlorite-like phases. At temperatures > depicted in Fig. 3-4 and discussed above, samples 373 K, oxygen isotope exchange reactions would subjected to thermal sterilization might also suffer occur at significant rates for clay minerals and destruction of any fluid inclusions, resetting of related silicates (O'Neil, 1987). mineral geothermometers, and annealing of radiation damage. 18

Behavior of fluid inclusions (usually water- very noticeable effects should be observable after based) in minerals during heating and refrigeration one day at 623 K (R. Walker and C. Naeser letters, can yield unique information concerning the Appendix A3). The latter treatment would degrade physical and chemical conditions under which the the information to be obtained but would not minerals formed. Heat treatment at < 550 K will totally erase it, especially in minerals from basaltic have relatively little effect except for incompetent and high-grade metamorphic rocks. and cleavable minerals, such as carbonates and Lower temperatures maintained for longer nitrates, which are expected to decrepitate at times would be equivalent to higher temperatures significantly lower temperatures in response to maintained for shorter times. For example, apatite internal pressures developed in the inclusions held at 498 K for 104 rain. (6.9 days) would also be (Roedder letter, Appendix A3). partly annealed (Naeser and Faul, 1969). Presence Mineralogical geothermometry uses of water vapor would markedly increase the track crystallographic states of certain minerals, or annealing rates. Further work is required on the elemental distributions between certain mineral kinetics of track annealing, especially in clay pairs, to deduce the temperature at which the minerals or other minerals of low-temperature minerals formed. Heat sterilization will negate origin. opportunities for thermometry if it modifies crystal In the context of natural TL, the lower structures or changes elemental distributions in the maximum surface temperatures on Mars, relative thermometer minerals. Temperatures of formation to the Moon, suggests that a much greater portion based on mineral structure or composition will not of trapped electrons should remain stored in be compromised if the assemblage does not change Martian samples. TL could be used on a Martian below the sterilization temperature, provided that deep-core sample for determining natural the threshold for change is not markedly affected radiation-shielding depths in the material and by the nature of the vapor phase in equilibrium potentially for derivation of planetary heat flow with the assemblage. The thermometer minerals (Arvidson letter, Appendix A3). TL would be most resistant to heat modification are those with adversely affected by any heat treatment > 373 IC low diffusivity, high hardness, and high melting

points. Therefore, mineral assemblages in igneous Table3.6. Temperatures (K) for which one-hour heat or metamorphic rocks are likely to survive, treatment anneals nuclear particle tracks provided that the vapor phase is not greatly different from that present during the history of the assemblage on Mars. Those minerals most 373 Basaltic glass (MacDougall, 1973) amenable to geothermometrie methods are Lunar impact glass (Fleischcr et al., 1971) silicates, transition element oxides, sulfides with high melting points, and anhydrous carbonates. 473 Feldspar glass (Fleischer et al., 1968) Those that would not provide geothermometric Basaltic glass (Fleischer et al., 1969) information after sterilization are hydrated minerals, oxysalts, and sulfides with low melting 573 Apatite (Naeser and Faul, 1969) points. Lunar impact glass (Fleischer and Hart, 1973) The extent of heat sterilization of a returned sample would markedly affect the amount of 673 Phlogopite (Maurette et al., 1964) information that could be gained from cosmic-ray- Muscovite (Fleischer et al., 1964) induced or fission-induced nuclear particle tracks or from radiation-induced thermoluminescence 773 Pyroxene (pigeonite) (Fleischer et al., 1965a) (TL) (Section 3.5). The ease of annealing of tracks Olivine (Fleischer et al., 1965b) within a mineral is proportional to rates of self-diffusion of elements within the mineral. As a 873 Sphene (Naeser and Faul, 1969) general rule, the harder a mineral and the higher Diopside (P.B. Price, Appendix A3) its decomposition temperature, the greater its Epidote (Naeser et al., 1970) resistance to track annealing. Heating would also Garnet (P.B. Price, Appendix A3) free trapped electrons, thereby erasing natural TL. A summary of track annealing temperatures is 973 Zircon (Fleischer et al., 1965b) listed in Table 3.6. Large annealing effects should Feldspar (Fleischer et al., 1965a) not be noticed in most minerals below 423 K but 19

3.4. Pressure

At a constant temperature, increase in / confining pressure associated with Martian samples (3_ 7 mlb Mars 1 / _-_16 i G tmo sp here _ // can cause adsorption of gases whereas a pressure Nontronlte, decrease can cause gas desorption. Either process ,,_.u12 I. 158 K will almost certainly alter the character of the gl0i sample relative to its state when collected. o No nb-o n_t.e. o 8 bJ Basalt, 196 K Sufficiently high increases in pressure can drive 1 5B K Nontronlte, _6 chemical or isotope-exchange reactions that might I 250 K_ irreversibly change the natural character of the 196

sample. Accordingly, preservation of Martian 222--:- ...... Ot samples must address both the total pressure and 0 1 2 composition of head-space gases in contact with the Lag P(C02_ ([orr) samples.

Atmospheric pressure at the Martian surface Figure 3-6. varies with both elevation and season. At low

elevations such as the two Viking landing sites, the CO 2 gas adsorption on powdered samples of Mars- seasonal range lies between about 6.5 mb and 10 analogous geologic materials as a function of mb (Fig. 3-5). The chemical composition of the temperature (modified from Fanale and Cannon,

near-surface Martian atmosphere is mostly CO 2 1979). The vertical dotted line represents a typical

with traces of N2, Ar, 02, and H20 (Table 3.3). partial pressure of CO 2 in the Mars atmosphere. The major source of pressure rise would probably be desorption of gases during warming of water vapor (Fanale and Cannon, 1974) as well as a Martian sample in a sealed container. noble gases (Fanale and Cannon, 1978). The Laboratory experiments have shown that, under general trend, as shown in Fig. 3-6, is for increasing simulated Martian conditions, large quantities of adsorbed gas load with decreasing temperature. gaseous CO 2 can be adsorbed on reasonable Accordingly, time-grained soils and sediments on geologic analogs of Mars surface materials (Fig 3- Mars are expected to contain substantial quantities 6). The same materials can also adsorb substantial of adsorbed gases prior to collection. Two useful end-member materials for gas adsorption/desorption studies are powdered basalt and powdered smectite clays. As reviewed in

10 Summer /_ Summer I Chapter 2, mafic igneous rocks akin to basalts are expected to comprise a large proportion of the ,Fall Spr_ng g Martian crust. Chemical alteration and weathering of those marie rocks is expected to produce various free-grained, volatile-bearing phases, possibly \ including smectites or smectite-like mineraloids. Smectites, in particular, are known to have very 7 large specific surface areas and strong gas Sol_tlce adsorptivities. Powdered basaits possess only , i , i i i i b i i i J modest specific surface areas and adsorptivities and 0 IO0 200 30g 4,00 _,00 600 700 VL-I SOLS can be considered a baseline model for a particulate regolith on Mars. Using knowledge of desorption characteristics, Figure 3-5. the pressure rise as a function of temperature for a sealed sample can be readily computed. Fig. 3-7 Seasonal variation of atmospheric pressure at the summarizes pressure rises expected for the Viking landing sites (modified from Hess et al., hypothetical cases of basalt and nontronite (ferroan 1980). The gap in the VL-2 curve reflects absence of smectite) regolith samples. Initial CO 2 loads are available data from the Lander. Other smaller gaps taken from experimental data (Fig. 3-6) have been artificially smoothed out in both the VL-1 corresponding to a 7-mb Martian atmosphere and VL-2 curves. whereas initial H20 loads are estimated from basic 2O mineralogicalpropertiesandcommonexperience. 100, Naturally,effectivehead-spacepressureswould I PRE55LJRE FROM DESORSED C02 I varywiththevolumeofthecontainer,theweightof I 500 g SAMPLE IN 1000 crn3 CONTAINER solidsample,and the degassinghistoryof the .,°I sample prior to sealingin the container. Nonetheless,resultsdepictedin Fig.3-7pointout themagnitudeof pressureriseto beexpectedfor ! _ E, Rr; ..... 2:;: ...... gasdesorptionfromcoldregolithsamples. J z_ ..... ---- i 1, / .I .... co-z-_-._zsr_/ Fig.3-7posestwohypotheticalcases:warming o.1!- /,' / / l_e K no,olt" 1.'_ of t'me-grainedsamplesoriginallygas-saturatedat 1,' // .o..,oo,,. 158K and230K, respectively.The158K case // /,' // 2.30K a,,,t 0., wouldapplyto samplescollectedfrompolarareas :,oo ._,oo ,oo . oo whereasthe230K casewouldapplyto samples collectedfromdepths> 25cmat equatorialand temperatelatitudes(Section3.3). ' Beginningat Marsatmosphericpressure(0.01 ,OOL,000o,.,.,3CONT,,NE,f I atm)andusingthe7-mbdatafrom Fig.3-6 to model CO2 desorption with increasing temperature,it isfoundthat,by230K, head-space pressureabovebasaltand nontronitesamples i ...j,,,, I initiallygas-saturatedwithCO2 at 158K are0.56 ' ...... / / ,,_'- k' CO2 cm-_ 5rP/g .q. X HzO I atmand6.0atm,respectively.If allCO2desorbs t ,' l/# l_a K no,o,, ,._ 1 I o.1 I,,11_,<,0,,_. _2_._ zo I by 300K, respectivepressuresbecome0.98atm MARS // t 2'10 X Bagoli 0.4 I / and9.1atm. Above300K, pressureincreasewas 2_10 K No_ronitl 1 g 2'0 modelledaccordingtotheidealgaslaw. _00 200 300 400 5O0 It is assumedthatno H20 desorptionoccurs TEMPERATURE (K) below230K sothatpressurerisebelow230K is attributablesolelytoCO2desorption.(Additional Figure 3-7. pressurefromdesorbedN2 andAr is neglected.) Above230K, desorptionof wateris expectedto Head-space pressures developed by desorption of becomeimportant.Forbasalt,aninitialwaterload gases from Mars-analogous materials inside a fixed of1%wasassumedtodesorbto0.1%by300K and volume. (Top) Desorption of CO2, modelled using to0.01%by400K. Consequently,at300K, the data from Fig. 3-6. (Bottom) Total pressure from partialpressuresof gasabovetheinitiallycoldest desorption of CO2, as above, plus desorption of basalt(158K)wouldbe0.98atmCO2and7.4atm H20 estimated from mineralogical properties. H20. Usinganinitialwaterloadof 20%for the initiallycoldestnontronite(158K),with18%being retainedon thesubstrateupto 300K, equivalent chemical or isotope-exchange reactions. At least one of the oxidants discovered in resultswere9.1atmCO2and18atmH20 at300 K. Forthecaseof samplesgas-saturatedat230K, Martian sediments by the Viking Landers is known correspondingtotalpressuresat 300K wouldbe to decompose, with voluminous release of 0 2, 19.5atm for nontroniteand7.6atm for basalt. upon humidification (Oyama and Berdahl, 1977). Basedonlaboratoryexperiencewithclayminerals, Desorption of water vapor from a sealed sample majordesorptionof waterfrom nontronitewas could humidify the container and decrepitate the assumedtooccurat300-400K. subject oxidant. To minimizepressurerise,gas-richsamples Stable-isotope exchange reactions under the musteitherbekeptextremelycold(i.e.,< 230K) subject conditions (low T, high P) have not been or degassedprior to sealingin containers. extensively studied but, from the law of chemical Althoughmodeldesorptionprofilesfor H20 mass action, any increase in Pc02 or PH20 should shouldbe measuredprecisely,it alreadyseems foster increased rates of 13C/12C and 180/160 clearthatpressuremanagementshouldbe more exchange reactions, respectively. Such reactions difficultfor CO2 + H20 than for CO2 alone. could irreversibly change the stable-isotopic Head-spacegas pressureshouldnot exceed compositions of any carbonate or hydrated thresholdsfor materialdecompositionor for minerals in the sample. 21

3.5. Ionizing Radiation By-products of GCR (and SCR) bombardment, especially secondary gamma The cosmic-ray bombardment records radiation, also produce electron-hole damage that preserved in the surfaces of Martian rocks are forms the basis of the TL effect. Radiation expected to provide valuable information about received by the sample leads to electrons being variations in density of the Martian atmosphere trapped in energy levels in the "forbidden" band gap through time (Arvidson et al., 1981). Also, of the solid. Ambient temperatures on the planet radiation damage accumulated in samples through can cause some of the electrons to be released cosmic-ray bombardment and through in situ decay from these traps. By studying the increase in of natural radionuclides can be used to age-date trapped electrons, in response to radiation intensity the samples through the method of and energy release upon systematic heating, thermoluminescence (TL) (e.g., Wendlandt, 1986). information on radiation-f'dling and thermal Care must be taken, however, to minimize effects drainage should be obtained. From these studies, of irradiations experienced by samples outside their natural environments after they are collected. Such extraneous irradiations might obscure the natural records that are sought in the samples. Concerns I _ I L Ar--39 about preservation of natural irradiation records in Mars samples were expressed in letters by P. I _ / ...... \ 8 i _ _ \ Englert and by R. Reedy, W. Feldman, and D. Drake (Appendix B3). Cosmic radiation is subdivided into solar cosmic rays (SCRs) and galactic cosmic rays _-2 F \ ccR ,,I (GCRs) (Table 3.7). The Martian surface is mostly _ I ,r_8 T .... /.--2 .... _ Track_l ,_l I ...... '...... 7 l,Y" :ll shielded from SCRs by the Martian atmosphere (2.6 g/em 2 shielding for each mbar of pressure), / 't_: glcm 2 which also provides differential shielding against -1 o 1 2 3 Lo¢:jSHIELDING DEPTH GCRs. GCRs consist of very heavy (VH) nuclei (Z > 20), which impart damage through ionization of Figure 3-8. target atoms, and free nucleons (protons and neutrons), which impart damage through nuclear spallation reactions. Products of GCR VH Production rates of radiation damage effects in Mars bombardment are microscopic cylindrical traces of surface materials as a function of shielding (modified from Arvidson et al., 1981.) Note that SCR effects crystal-structure damage that become visible as become important for shielding < 5 g/cm 2, which is "tracks" in polished grain mounts after suitable chemical etching. Products of spallation include equivalent to 2 mb of Mars atmosphere. Under current climatic conditions, with a typical noble-gas nuclides (e.g., 39mr, 78Kr, 83Kr) that must atmospheric pressure of 7 rob, most Mars samples be extracted from a sample by pyrolysis and measured with an ultrasensitive mass spectrometer. are protected from SCR track damage.

Table 3.7. Characteristics of solar cosmic ray (SCR) and galactic cosmic ray (GCR) components (after Reedy et al., 1983)

Energies Mean flux at Earth Penetration Depth Radiation (MeV/nucleon) (particles/cm2/sec) in Rocks (cm)

SCR protons and He nuclei 5-100 - 1130 0-2 SCR very heavy (VH) nuclei 1-50 - 1 0-0.1

GCR protons and He nuclei 100-3000 3 0-100 GCR very heavy (VH) nuclei - 100 0.03 0-10 22

gamma-ray equivalent dose of radiation can be to the recoverable information. Production of determined and, hence, a radiation history can be tracks and spallation products in bulk meteorite obtained for a given sample. The technique has samples irradiated in interplanetary space are been applied successfully to lunar samples and ordinarily considered as occurring on time scales of meteorites. One of the most important kinds of 106-107 yr. For a planetary surface sample, information that can be obtained from TL studies however, actual measurements may depend on is the depth of burial of a sample below the surface; individual mineral grains that could be perturbed this can be calculated from the determination of by even short-rived fluxes of extraneous radiation. the effective storage temperature for the electron In addition, irradiation effects can vary greatly with traps. Penetrating radiations seriously affect data depth in a sample. For example, in the outermost that can be obtained. Even exposure to visible light 10-3 cm of a mineral grain with no atmospheric degrades results, and sampling is done ideally in shielding, the VH-nuclei track production rate red light (R. E. Arvidson letter, Appendix A3). could be as high as 105 cm "2 yr "1 (Fig. 3-10) (Reedy The Martian atmosphere effectively shields et al., 1983). Because the elapsed time between against VH nuclei but not against nucleons. collection and Earth-delivery of a Mars sample Therefore, the abundance ratio of tracks to might be one year or longer, extraneous track spallation products should be sensitive to variations production in improperly shielded samples could in density of the Mars atmosphere (Fig. 3-7). In accrue into a major fraction of the total measurable fact, for an atmospheric pressure change from 1 to track population in a given grain. Similarly, in the 100 mbar (i.e., change of 3 to 300 g/cm 2 shielding), absence of atmospheric shielding, production rates the track/spallation-product ratio changes by five of spallogenic 1°Be and 26A1 within the outermost 1 orders of magnitude (Fig. 3-9). Because relative cm of a rock would be approximately 101"3 decays production rates for tracks and spallation products kg-I min -1 (Fig. 3-10). SCRs are especially are so sensitive to shielding (Figs. 3-8, 3-9), major important in production of 26A1 and might become changes in the shielding history of a sample, during significant once a Mars sample was rifted above the collection and return to Earth, could pose a threat SCR shielding provided by the Mars atmosphere.

20, (rrocks/cm2)/(cm3 srP/g) 4, _VH Tr<3cks _"_ AI 26 Co-60

Relative Rates _. ct Surfoce < _ 17

.£ ,.,,\ i Z,o_,,/c,_2 y, /' \"-,. co_s6 / o, - fro., X-,.z I Deep Regollth \\ X DeccWs/kg-yr _\ / , '\ X .rnD _2 [ N.. cm/ I¢ -3 -2 -1 0 1 2 o 1 Log DEPTH Log SURFACE PRESSURE

Figure 3-9. Figure 3-10.

Production rates for tracks and spallation nuclides Relative production rates of track damage and calculated for a lunar basaltic rock directly exposed spallation 78Kr at the Mars surface (e.g., free surface of a rock) and in the deep regolith (modified after to SCRs and GCRs (no shielding) The shaded area reflects uncertainties in fluxes of low-energy SCR Arvidson et al., 1981). The strong dependence of the track/spallation-gas ratio on atmospheric shielding VII nuclei (modified after Reedy et al., 1983). forms the basis of climatology information in sample Similar rates should apply to Martian rocks. Note that the unshielded outermost surface of a rock irradiation records. The deep-regolith curve

represents the same ratio from the bottom of the would accrue significant damage over the 1-2 years atmosphere to a depth within the regolith that that might typify surface-operation and Earth-return exceeds the penetration range of GCRs. phases of a Mars sample-return mission. 23

Radiation-shielding requirements for Mars 3.6. Magnetic Fields samples are traceable to two major concerns: Permanent magnetization of Martian rock Naturally well-shielded samples taken from samples will be sought as evidence for ancient depth on Mars (e.g., > 10 cm) will be exposed planetary magnetic fields on Mars. Therefore, any to high doses of GCRs upon excavation. degradation or obscuration of natural magnetization in the samples will be viewed as a All Mars samples, regardless of depths of significant loss of paleomagnetic information. The origins, will be exposed to high doses of SCRs samples must be protected against events that (or their secondary products) after liftoff from might either erase natural magnetization or induce Mars. artificial magnetization. Concerns held by specialists in rock magnetism are reflected in the GCR nucleons are very highly penetrating and letter by D. Collinson and A. Stephenson their stoppage requires shielding on the order of (Appendix B3). 1000 g/cm z (Fig. 3-8) -- a value that is extremely Both heating and shock are known to be impractical in weight-limited spacecraft systems. deleterious to remanent magnetism in rocks and Furthermore, moderate to large shielding depths should be avoided. The maghemite/hematite levied against - 1 GeV nucleons (aside from those solid-state phase transition, which can occur over needed for complete stoppage) become self- the 350-650 K range for various samples (Fig. 3-4), defeating. GCR bombardment of the shield can be avoided by keeping the samples cold. material produces cascades of secondary nucleons Altered magnetization is a serious concern if that impart additional radiation damage. Indeed, the samples are heated at temperatures in a mass-limited shielding environment, total approaching those for biological sterilization. First, radiation damage from GCR nucleons is minimized some material may acquire a non-Martian by minimizing shielding. magnetization when heated and cooled in the Total shielding cannot be "zero", however, presence of a magnetic field. For example, because some protection must be provided against goethite magnetizes on cooling from above 393 K the less energetic, but still damaging, primary and troilite magnetizes on cooling from above 593 SCRs. As shown in Fig. 3-8, contributions by SCRs K. Second, it may be impossible to heat the to heavy-nuclei track damage becomes significant samples significantly without changing the magnetic only for shielding less than 5 g/cm 2. At higher carrier. For example, the reaction goethite---, shielding values, no additional protection against hematite occurs at 473-623 K in air and the SCRs is gained but additional complications are alteration of fine-grained or amorphous iron oxides incurred through rapid changes in the can occur at temperatures significantly less than track/spallation production rates and in increasing 623 K. In addition, any carbon-induced reduction secondary damage from GCRs. Accordingly, all reactions might produce ultrafine-grained metallic factors considered, a baseline shielding value of 5 iron that might acquire magnetization at g/cm 2 is recommended for collected Mars samples. temperatures < 423 K. Coilinson and Stephenson It should be understood that 5 g/cm z (Appendix B3) suggest that a temperature of 373 K represents the total shielding, including and an ambient magnetic field strength of < 10-4 contributions from containers and spacecraft Tesla could be tolerated without significant change structures. When container and spacecraft effects of natural magnetism. are considered, along with effects of adjacent The best strategy for preserving natural samples, additional dedicated shields may be magnetization of Martian samples is to keep the unnecessary. Indeed, the minimum structures samples cold and shielded from artificial magnetic required to containerize and transport samples fields. The important issue, requiring carefully during Earth return might contribute shielding > 5 planned analog studies, is to understand clearly the g/cm z. In that case, neutron absorbers (e.g., B, Li, magnetic overprinting that might occur by heating a Cd) might be desirable additions to hardware sample significantly above the Martian surface surrounding the samples to reduce secondary temperature. Care should be taken to insure that radiation from GCRs. In any event, either passive the samples are not exposed to magnetic fields, on or active monitors of ionizing radiation would be the spacecraft or on the return to Earth, which are desirable sensor companions to the samples. significantly stronger than Earth's magnetic field. 24

3.7. Acceleration and Shock

Physical properties of interest for Martian I I FOR MARTIAN SAMPLES regolith samples include particle-size distributions, _AR5 GRAV IY ] [Comi_ared wit_ V_Wing Mote?iol I porosities and permeabilities, zonal structures that _" " t " - [ Cohesion:I) J vary with depth, and intergranutar cementation, as EARTH GRAVITY in duricrusts observed at the Viking Lander sites. i s_mpl4 = _ _'cr_ I As expressed in the letter from E. Gaffney ! ,o_-oNo:,

(Appendix B3), the principal threats to the i i ..:._.i_._s._._.z-_a_-.-.i--.-_-_ preservation of such properties are high

acceleration (sustained g-force loads) or shock o _*"1

(short-lived, high-intensity pressure) that might 2 4 B B 10 12 break grains, sever grain-to-grain contacts, or cause N,:j mixing or compaction. Additional concerns are that shock might degrade natural magnetization of Figure 3-11. samples (Collinson and Stephenson, Appendix B3). Stress (directed pressure) experienced by a Acceleration-force milestones for Martian samples. bulk 1-gram sample, as a force normal to the face Positively sloping straight lines represent stress of a cube, can be estimated as computed as a function of "g" number (where 1 g = 981 cm/sec 2) for unit-mass (1 gram and

S = 98.1Ng d2/3 [3-2] approximately 1--cm size) sample materials of various densities. The horizontal lines show average values

where S (Pa) is stress, Ng is the "g" number (1, 2, 3, of the strengths of blocky, crusty/cloddy, and drift etc.) of the acceleration (Ng = 0.385 at the material at the Viking Lander sites as estimated by Martian surface) and d is the specific gravity Moore (1987). (normalized bulk density) of the sample Stresses computed as a function of g-load using Eqn. [3-2] strength estimated by Moore (1987) for three types of surface materials observed at the Viking Lander are shown in Fig. 3-11. sites. The two weaker materials ("drift" and Fig. 3-11 offers a simplified summary of acceleration-induced stresses on samples but must "crusty/cloddy") probably also have low densities (d be qualified by consideration of sample size and < 2). From Fig. 3-11, it is apparent that unit-mass geometry. Samples in elongated containers (e.g., (approximately 1-cm-sized) samples of drift or regolith core tubes), will experience compression crusty/cloddy materials would fail for stresses from acceleration of material along the length of greater than about Ng = 7-11. Average blocky material should be resistant to stress-induced the sample column; sample increments at the forward end of the acceleration vector will failure at all accelerations Ng < 35 for d = 2. Of experience higher stresses than those near the tail course, S varies with L and there remain large of the vector. Accordingly, compression at the uncertainties in the strengths estimated for all three bottom (trailing end) of the tube is estimated materials classified by Moore (1987). better as Values of Ng required to assure survival of the very weak drift and crusty/cloddy materials are S = 98.1 Ng d L [3-3] exceedingly low and might be impractical as mission requirements. Given the range of to account for the effect of length, L. (For unit- strengths estimated for blocky material, however, it mass samples modelled by Eqn. [3-2], L< 1 cm is seems that a centimeter-sized blocky material implicit.) Clearly, stresses will be highest when sample could be preserved for all Ng < 10. The stress limit of < 1 kPa suggested by Gaffney acceleration is parallel to L. Stress management might be achieved by minimizing L for each sample (Appendix B3) would translate to about Ng = 7 for and by preferentially orienting L transverse to the a unit-mass sample of d = 2. Taking the length acceleration vector. effect (Eqn. [3-3]) into account, however, a 7-g The important consideration is whether acceleration applied to a 10-cm columnar sample of computed stresses exceed strengths estimated for d = 2 would produce a 13.7 kPa load at the bottom Martian regolith materials. The horizontal dotted of the column, thereby threatening the integrity of lines in Fig. 3-11 show the average values of even the blocky material. 25

Assessing the acceleration/shock threat to radiation shielding required for biology would be rocks is simpler than for unconsolidated regolith greater than for geochemistry. Protection from samples. Crushing strengths of most terrestrial light would not be peculiar to biological samples rocks are on the Grder of 107 Pa whereas major but would already be required for mineralogical transformations and melting occur thermoluminescence samples (Section 3.5). under shock loads of 101° Pa. For d = 3, In addition to threatening the chemical and corresponding accelerations on unit samples (Eqn. stable-isotopic integrity of the samples, [3-2]) would be Ng = 490 (rock crushing) to Ng = uncontrolled pressure rise within sample containers 4.9 x 105 (rock melting). Clearly, such might also jeopardize planetary protection. As accelerations would be totally unreasonable for any long as head-space pressures inside Mars sample sample-return spacecraft or mission design. containers are less than atmospheric pressure on With respect to shock disturbance of rock Earth, no leakage of gases into the terrestrial magnetism, Cisowski et al. (1976) experimentally environment should occur. If pressures inside determined that demagnetization occurs at shock containers exceed 1 atm, however, the pressure pressures < 109 Pa in basalt targets. It is not clear, difference will cause net diffusion of Mars gases however, whether the threshold for such effects is outward through all available leakage pathways. much less than 109 Pa. Therefore, protection of Any putative biohazard posed by the Martian rock samples against shock-induced crushing (i.e., samples would thereby become much more difficult 107 Pa) should also be adequate for magnetic to manage. Therefore, maintenance of minimum, preservation. Nonetheless, additional work may Mars-like head-space gas pressures (Section 3.4) is still be needed to define shock limits for magnetic also highly desirable from the perspective of preservation of soil or sediment samples. planetary protection.

3.8. Biology and Planetary Quarantine 3.9. Summary

Preservation of the most sensitive geologic General concerns about preservation of Mars materials should also suffice to preserve any non- samples are summarized in Fig. 3-12. Details of living Martian biological materials (i.e., organic or various issues wer_ reviewed in Sections 3.2-3.8. biochemical compounds). Accordingly, biological The maximum scientific value of the samples is concerns would require few, if any, stipulations in retained when the samples are preserved in the addition to those discussed in sections 3.2-3.7 conditions that applied prior to their collection. except in the unlikely event that return of living Unfortunately, all manipulations of the samples, organisms became an objective. As reviewed including collection and containerization, can be previously (Section 2.1.4), however, principal expected to degrade the samples to some extent. emphasis in Martian exobiology is aimed at Design of meaningful sample-preservation returning well-preserved samples of any Martian precautions must recognize how and why samples organic compounds. become degraded if environmental controls are Contamination by carbon would be offensive to relaxed. biological studies but the - 40-ppm C background Avoidance of contamination is an absolute level expected for sterile rock samples (Section 3.2) necessity although quantitative limits vary from one might represent a practical limit to biological anti- chemical element to another. The bulk elemental contamination. Sub-freezing temperatures and low composition of shergottite meteorites might serve head-space gas pressures should favor survival of as a guide for setting maximum acceptable limits of biochemical compounds by arresting reactions that elemental contaminants. Prospective tool and might otherwise decompose them. Protection of container materials rich in trace elements (by the soil clods against acceleration/shock disintegration shergottite definition) should be scrupulously should also protect any microfossils. Shielding avoided. against extraneous magnetic fields, as required for Temperature is the most important intensive paleomagnetic studies, might be unnecessary for parameter to control. Keeping the samples biology but should not be offensive to biology. sufficiently cold will immobilize water (as ice or as Only the shielding requirements against ionizing adsorbed water vapor) and prevent chemical and radiation might be expected to differ for isotope-exchange reactions that could otherwise geochemistry and biology. If anything, the irreversibly change the records of natural history in 26

the rocksandsoils. Strict temperaturecontrol wouldalsomoderatethe desorptionof gaseous ENVIRONMENTPOSSIBLE ONEFFECTSMARS SAMPLEOF UNCONTROLLEDPRESERVATION i CO 2 and H20 from l'me-grained soils and sediments that could lead to unacceptably high head-space gas pressures inside sample containers. CONTAMINATION • Extnaneous element/compound precludes measurement Uncontrolled pressure rise would decompose of native Mcrtlon chemical or isotopic composition

pressure-sensitive materials, such as the trace TEMPERATURE oxidants discovered in surface sediments at the • Mo_illzecl *_ter s_cts irreversible chemical reactions

Viking landing sites, as well as encourage chemical • Heet-sensit_ve materiels decompose and isotope-exchange reactions involving any • unidentified oxidants discovered by Vik;ng Lenders • _n;neral and stoble-isotop;c records of carbonate or hydrated minerals. Deliberate cnc;ent Mars cl[rnetes

thermal sterilization of samples would irreversibly • N(3t.ural radiation dos[reeLers erased by anneol[ng decompose heat-sensitive minerals, alter stable- isotopic ratios, and possibly erase records of •, PRESSURE (HEAD-SPACE ,GAS) • Unr_turol pressure and humidity couBe irreversible natural radiation doses that would be critical to chemical and [sotopic--exchancje reactions paleoclimate studies. • Pressure-sensitive compounds decorn_ose

Management of ionizing radiation doses, • iONIZING RADIATION

exposure to extraneous magnetic fields, and • Natural Mars radiation history is erased or obscured subjection to high accelerations (including shock) (_mclud;ng clirna+-e-chonge records) are also important but more difficult to express as • MACNETIC FIELDS quantitative limits that apply uniformly to all • Natural Viers rnotjnetic h;story is eroseCl or obscurec_ • Extraneous mognetlzotlon ;s ;nduced as a_focts samples. Protection against ionizing radiation is • ACCELERATION AND SHOCK most critical for geologic samples (as opposed to • Phys[cal properties degraded for salt clods atmospheric samples) taken from depth (i.e., a few (porosity, permeahility, ;nter--cJroln structures, centimeters or more), whereas magnetic shielding cementation) is principally a concern for igneous rock samples. Acceleration/shock limits are of concern only for Figure 3-12. deep regolith samples and for partially cemented sediments or soil clods. Summary of major concerns regarding preservation By observing preservation requirements for the of collected Martian samples. most sensitive geologic materials, preservation of any organic or biochemical materials should also be achieved with no additional effort. Preservation requirements for geologic and organic materials are mutually supportive. Although many consequences of uncontrolled environment on Mars sample preservation can already be identified, basic research is still needed in several areas prior to specification of firm preservation requirements. In addition, work is needed to establish what scientific measurements can be made on Mars to recover information that is unlikely to be preserved in returned Martian samples. Recommendations both for preliminary preservation requirements and for additional work are given in Chapter 4. 27

4. RECOMMENDATIONS ]

Preliminary values for sample-preservation Elemental composition of the Martian parameters are summarized in Table 4.1. Those atmosphere is known from analyses by the l,qking values were derived using background information Landers. It is suggested that, for each element, that was explained in detail in Chapter 3 but are contamination of an atmospheric sample not subject to modification based on future research. exceed 1% of the concentration in the Vikhtg Specific reasoning involved in compiling Table 4.1 analyses. For example, using data in Table 3.3, is given below. derived limits would be < 0.03 % N 2 and < 0.8 Contamination. High-purity aluminum and ppb Xe. Research is needed to show how certain stainless steel alloys should be acceptable contamination of atmospheric samples varies with materials for sample tools and containers. Other method of sample collection. Volumes collected materials may be acceptable if they can be certified and stored at Mars ambient pressure should be as non-contaminating with respect to trace representative samples but would be subject to elements of geochemical interest. Research is contamination on Earth by inward leakage of the needed to certify prospective materials as non- terrestrial atmosphere. Concentrated samples reactive with oxidants of the type discovered in (e.g., collected by compression or sorption on Martian sediments by the Viking Landers. molecular sieves) would be less sensitive to The Shergotty meteorite, which has been terrestrial contamination but might be either postulated to be a Martian rock, has been fractionated or contaminated by the concentration extensively analyzed and is a useful guide to process. acceptable upper limits for contamination of rock, Cross-contamination between individual soil, and sediment samples. It is suggested that, for samples should be minimized by separately each element, contamination not exceed 1% of the packaging different samples. concentration in Shergotty. For example, using Chemical sterilization would introduce severe data in Table 3.2, derived limits would be < 0.5 chemical and isotopic contamination and should be ppm C and < 0.9 ppb Pb. avoided.

Table 4.1. Recommended parametric values for preservation of Martian samples. (Unless otherwise noted, each stated limit applies equally to every sample). See text for limitations and qualifications.

Contamination For each element, < 1% of the concentration in Shergotty meteorite (Rock, sediment, or soil sample)

For each element or compound, < 1% of of the concentration in

Viking Lander atmospheric analyses (Atmosphere sample)

Temperature < 260 K (Igneous rock sample, unweathered)

< 230 K (Soil, sediment, deep regolith, or weathered rock sample)

Pressure (head-space gas) < 1 atm (Igneous rock sample, unweathered)

< 0.0l arm (Soil, sediment, deep regolith, or weathered rock sample)

Ionizing Radiation 5 g/cm 2 shielding

Magnetic Fields < 5.7 x 10 -5 Tesla (1 Earth field)

Acceleration/Shock < 7g(lg = 9.81m/sec 2) 28

Temperature. Temperature is the most generate significant head-space gas pressures. The important intensive variable to control. problem will be least for rocks and greatest for Preservation temperatures should be established fine-grained soils and sediments and, especially, with the goal of controlling the physical state and deep regolith samples. The latter samples are also reactivity of water. Immobilizing water in the expected to be the most sensitive with respect to samples as ice, or as unfrozen capillary films that pressure-induced chemical or isotope-exchange are thinner than the threshold for liquid-like reactions. behavior, will minimize chemical and stable-isotope Research is needed on the rates of reactions involving carbonate and hydrated minerals with exchange reactions. The equilibrium freezing point of 273 K is too gases containing high partial pressures of CO 2 and warm to assure control of the water system. The H20. Such work might reduce concerns about onset of liquid-like unfrozen water in rocks occurs deleterious effects of pressure and permit higher at 263 K and, in clay-rich soils, at about 235 IC pressure tolerances to be derived. In advance of the necessary research, however, Therefore, it is recommended that fresh igneous rocks be preserved at < 260 K and that samples a pressure limit of 0.01 atm (effectively Mars containing clay-like minerals or mineraloids be ambient) is recommended for most geologic preserved at < 230 K. samples. A maximum limit of 1 atm is suggested not on the basis of geochemistry but in anticipation Supporting research is needed on kinetics of geochemical changes, especially stable-isotope of planetary quarantine requirements. Pressure < 1 atm inside a sealed container will assure that, on exchange reactions. Also, work is needed to establish the survivability of natural Earth, no outward leakage should occur. thermoluminescence in Martian samples as a Ionizing Radiation. Shielding of 5 g/cm 2 function of preservation temperature. corresponds to the minimum value needed to Thermal sterilization at 400-450 K would prevent nuclear particle track damage from solar decompose sensitive minerals and compounds cosmic rays. (The Martian surface is naturally known or suspected to occur in Martian samples. protected from such effects by atmospheric Studies of igneous minerals and radiometric age- shielding). This shielding requirement is modest dating should not be affected but records of climate and might be achieved by default in a well-designed history would be seriously degraded, if not sample canister with self-shielding accrued through destroyed. In addition, mineral geothermometers strategic placement of samples relative to the and fluid inclusions would be adversely affected. canister's center. Care must be taken not to If thermal sterilization becomes required, it inadvertently create greater shielding, however, should be done at the lowest possible temperature because, for some radiation effects, shielding > > 5 with complete retention of any liberated gases. g/cm 2 stimulates secondary radiation damage from Time of sterilization, within reason, has much less galactic cosmic rays. Radiation monitors should effect on mineralogical properties than increased accompany the samples. Magnetic fields. Magnetic shielding temperature. It is of paramount importance to measure and record the time-temperature-pressure requirements are among those most poorly defined. Research is needed to establish the conditions during any sterilization. Much information contained in the pristine sample might combinations of applied field strength, thus be recovered. A sealed liner of high-purity temperature, and shock that can be tolerated without disturbance of magnetic records in the gold might be required to manage the loss of hydrogen and its associated effects on the redox samples. Spacecraft design and mission operations conditions of the minerals. Clearly, requirement must be analyzed to understand the artificial fields for a gold lining would need to be carefully to which samples might be subjected. In the balanced against limits for Au contamination. meantime, the limit for extraneous applied fields is No water or any other components should be set equal to that of Earth's field. Acceleration and Shock. No reasonable added to the sample for the sterilization process. accelerations or shocks expected during a Mars Although water might help preserve some clay minerals and zeolites, these potential benefits do sample-return mission should adversely affect not begin to offset the disadvantages of acclerated igneous rock samples. The 7-g limit corresponds to the stress that would disintegrate Martian materials chemical reactions involving other phases. Pressure. Because of gas desorption from the having the average cohesion of crusty/cloddy samples, warming of sealed containers will material at the l/iking landing sites. 29

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Wright I. P., Carr R. H., and Pillinger C. T. (1986) Carbon abundance and isotopic studies of Shergotty and other shergottite meteorites. Geochim. Cosmochirn. Acta., 50, 983-991. APPENDIX A1

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APPENDIX A2

APPENDIX A2 A2- I

CONTRIBUTORS TO JSC (1974)

According to the copies of correspondence included in JSC (1974, Appendix I), the individuals listed below contributed ideas and information that served as the basis for the 1974 report. For some of the contributors, affiliations in 1987 were different from those in 1974. In each case, the contributor's name is printed as it appeared on the signature line of the letter and the listed affiliation is that last known as of 1987.

Duwayne M. Anderson Texas A & M University Raymond E. Arvidson Washington University, St. Louis S. W. Bailey University of Wisconsin A. E. Bence Exxon Production Research Co., Houston, Texas D. A. Cadenhead University of Buffalo, New York Michael H. Carr U. S. Geological Survey, Menlo Park Raymond Davis, Jr. Brookhaven National Laboratory, New York Bruce R. Doe U. S. Geological Survey, Reston R. H. Dott University of Wisconsin, Madison Samuel Epstein California Institute of Technology Fraser Fanale University of Hawaii Robert O. Fournier U. S. Geological Survey, Menlo Park Clifford Frondel Harvard University Michael Fuller University of California, Santa Barbara Robert M. Garreis University of South Florida Gordon Goles University of Oregon Gilbert N. Hanson State University of New York, Stony Brook Stanley R. Hart Massachusetts Institute of Technology Robert M. Housley Rockwell International Science Center, California John Hower (Deceased) formerly of Case Western Reserve University, Ohio M. L. Jackson University of Wisconsin, Madison Blair F. Jones U. S. Geological Survey, Reston lan Kaplan University of California, Los Angeles Keith A Kvenvolden U. S. Geological Survey, Menlo Park Michael E. Lipschutz Purdue University Kurt Marti University of California, San Diego D. McKay NASA/Johnson Space Center D. M. Mickelson University of Wisconsin, Madison Charles W. Naeser U. S. Geological Survey, Denver Tobias Owen State University of New York, Stony Brook J. J. Papike South Dakota School of Mines and Technology P. Buford Price University of California, Berkeley C. C. Patterson (Deceased) California Institute of Technology George W. Reed, Jr. Argonne National Laboratory, Illinois R. C. Reedy Los Alamos National Laboratory, New Mexico John H. Reynolds University of California, Berkeley Motoaki Sato U. S. Geological Survey, Denver A2-2 APPENDIXA2, con't

R. A. Schmitt Oregon State University J. William Schopf University of California, Los Angeles Brian J. Skinner Yale University Joseph V. Smith University of Chicago D. W. Strangway University of British Columbia, Canada M. Tatsumoto U. S. Geological Survey, Denver Robert M. Walker Washington University H. Wanke Max-Planck-Institut fur Chemie, Mainz, FRG S. H. Ward University of Utah G. J. Wasserburg California Institute of Technology David R. Wones (Deceased) formerly of U. S. Geological Survey, (Reston) APPENDIX A3

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APPENDIX B2 B2-1

ADDRESSEES AND RESPONDENTS* TO 1987 "CALL FOR INPUT"

NAME ADDRESS

William H. Abbott Dallas, TX 75265 Philip Abelson Washington, I)(2 20005 John Adams Seattle, WA 98199 Stuart O. Agrell Cambridge CB2 3EQ, U.K T.J. Ahrens Pasadena, CA 91109 Arden L. Albee Pasadena, CA 91125 Joseph K. Alexander Washington, DC 20546 E. Calvin Alexander Minneapolis, MN 55455 Hannes Alfven La Jolla, CA 92093 Lew Allen, _r. Pasadena, CA 91109 Judy Allton Houston, TX 77058 Edward Anders Chicago, IL 60637 Don L. Anderson Pasadena, CA 91125 Duwayne Anderson College Station, TX 77843 George W. Andrews* Washington, DC 20560 John Annexstad Bemidji, MN 56601 D.E. Appleman Washington, DC 20560 John T. Armstrong Pasadena, CA 91125 James R. Arnold* La Jolla, CA 92093 Gustav Arrhenius La Jolla, CA 92093 Raymond E. Arv_dson St. Louis, MO 63130 Lewis D. Ashwal Houston, TX 77058 John R. Ashworth Birmingham B47ET U.K. Howard J. Axon United Kingdom Philip A. Baedecker Reston, VA 22092 John R. Bagby Jefferson City, MO 65101 Sturgis W. Bailey Madison, WI 53706 Victor R. Baker Tucson, AZ 85721 K. Banerjee Minneapolis, MN 55455 Amos Banin Rehovot, 72879 Israel A. Bar-Nun Tel-Aviv 69978, Israel David J. Barbe[ United Kingdom Nadine Barlow- Houston, TX 77059 Virgil E. Barnes Austin, TX 78712 James E. Barrick Lubbock, TX 79409 J. Paul Barringer Princeton, NJ 08542 D. John C. Barru Cambridge, MA 02133 V.L. Barsukov Moscow, USSR Charles A. Barth Boulder, CO 80309-0392 Paul B. Barton, Jr. Reston, VA 22092 Charles Baskerville Reston, VA 22092 Abhijit Basu Bloomington, IN 47405 Raymond Batson Flagstaff, AZ 86001 Richard Becker Minneapolis, MN 55455 R. Beerbower Binghamton, NY 13901 F. Begemann 65 Mainz, Fed. Rep. of Germany Jeffrey F. Bell Honolulu, HI 96822 Peter M. Bell Worcester, MA 01608-1446 A. E. Bence Houston, TX 77252 132-2 APPENDIXB2, con't

NAME ADDRESS

Timothy M. Benjamin Los Alamos, NM 87545 William A. Berggren Woods Hole, MA 02543 John L. Berkley Fredonia, NY 14063 David Bermudes Boston, MA 02215 Robert A. Berner New Haven, CT 06520 L.F. Bettenay Perth, Western Australia 6000 N. Bhandari India Klaus Biemann Cambridge, MA 02139 Alan Binder Houston, TX 77058 R.A. Binns North Ryde, Australia 2113 David C. Black Moffett Field, CA 94035 , Thomas R. Blackburn Laurinberg, NC 28352 Douglas Blanchard Houston, TX 77058 Milton Blander Argonne, IL 60439 George E. Blanford Houston, TX 77058 Karl Blasius Pasadena, CA 91101 Robert B. Blodgett Corvallis, OR 97331 Arthur L. Boettcher Los Angeles, CA 90024 D.D. Bogard Houston, TX 77058 Bruce F. Bohor Denver, CO 80225 J.N. Boland Australia Jon Boothroyd Kingston, RI 02881 Janet Borg 91406 Orsay, France Penelope J. Boston Boulder, CO 80307 David J. Bottjer Los Angeles, CA 90007 A.J. Boucot Corvallis, OR 97331 Joseph M. Boyce Washington, DC 20546 William V. Boynton Tucson, AZ 85721 J. Platt Bradbury Denver, CO 80225 John Bradley Chicago, IL 60616 Garrett W. Brass Miami, FL 33149 Carol S. Breed Flagstaff, AZ 86001 Robin Brett Reston, VA 22092 G.A. Briggs Washington, DC 20546 Mexico, D.F. B.E. Britron , Philip E. Brown Madison, WI 53706 Kenneth Brown Moraga, CA 94575 Dale Browne Houston, TX 77058 Donald E. Brownlee Seattle, WA 98195 William E. Brunk Washington, DC 20546 Vagn F. Buchwald 2800 Lyngby, Denmark Raymond J. Bula* Madison, Wl 53706 Ted Bunch Moffett Field, CA 94025 Bonnie J. Buratti Pasadena, CA 91109 Kevin Burke Houston, TX 77058 A. L. Burlingame Berkeley, CA 94720 Donald S. Burnett Pasadena, CA 91125 R.G. Burns Cambridge, MA 02139 Joseph A. Burns Ithaca, NY 14853 Peter R. Buseck Tempe, AZ 85287 D. A. Cadenhead* Buffalo, NY 14214 Melvin Calvin Berkeley, CA 94720 APPENDIXB2, con't B2-3

NAME ADDRESS

A.G.W. Cameron Cambridge, MA 02138 J.R. Cann United Kingdom Ian S. Carmichael Berkeley, CA 94720 Michael Carr Menlo Park, CA 94025 William A. Cassidy Pittsburgh, PA 15260 Moustafa Chahine Pasadena, CA 91109 Sherwood Chang Moffett Field, CA 94035 Clark R. Chapman Tucson, AZ 85704 Stillman C. Chase Goleta, CA 93017 C.L. Chou Champaign, IL 61820 Philip R. Christensen Tempe, AZ 85287 Robert L. Christiansen Menlo Park, CA 94025 Roy Christoffersen Tempe, AZ 85287 Mark J. Cintala Houston, TX 77058 Stanley M. Cisowski Santa Barbara, CA 93106 Uel S. Clanton Las Vegas, NV 89114 Benton C. Clark* Denver, CO 80201 Roger N. Clark Denver, CO 80225 Pamela E. Clark Pasadena, CA 91109 Roy S. Clarke, Jr. Washington, DC 20560 Donald D. Clayton Houston, TX 77251 Robert N. Clayton Chicago, IL 60637 W. H. Cleverly Kalgoorlie, Western Australia 6430 Stephen M. Clifford* Houston, TX 77058 Preston Cloud Santa Barbara, CA 93106 Gary Clow Menlo Park, CA 94025 A.G. Coats Washington, DC 20053 Aaron Cohen Houston, TX 77058 Alvin J. Cohen, Pittsburgh, PA 15260 D.W. Collinson NEI 7RU, UK Jim Conel Pasadena, CA 91103 Guy Joseph Consolmagno Cambridge, MA 02139 Rex E. Crick Arlington, TX 76019 John R. Cronin Tempe, AZ 85287 G. Crozaz St. Louis, MO 63130 James A. Cutts Pasadena, CA 91101 Paul E. Damon Tucson, AZ 85721 E.J. Dasch* Corvallis, OR 97331-5506 D. W. Davidson Ottawa, Canada KIA OR9 Merton E. Davies Santa Monica, CA 90406 Don Davis Tucson, AZ 85719 Phillip A. Davis, Jr. Flagstaff, AZ 86001 Andrew M. Davis Chicago, IL 60637 Raymond Davis, Jr. Upton, NY 11973 Donald J. De Paolo Los Angeles, CA 90024 Rene DeHon Monroe, LA 71209 Donald DeVincenzi Washington, DC 20546 Peter Deines University Park, PA 16802 Jeremy S. Delaney New York, NY 10024 John W. Delano Albany, NY 12222 B2-4 APPENDIXB2,con't

NAME ADDRESS

Michael R. Dence Ottawa, Ontario Canada, KIA 0Y3 D. J. Des Marais Moffett Field, CA 94035 John Dietrich Houston, TX 77058 Robert S. Dietz Tempe, AZ 85287 Robert T. Dodd Stony Brook, New York 11794 Bruce R. Doe Reston, VA 22092 Thomas M. Donahue Ann Arbor, MI 48109 J. Allan Donaldson Ottawa KIS 5B6, Canada Robert H. Dott, Jr. Madison, Wl 53706 Robert G. Douglas Los Angeles, CA 90007 Eric Dowty New York, NY 10024 Darrell M. Drake* Los Alamos, NM 87545 Michael J. Drake Tucson, AZ 85721 Gerlind Dreibus 65 Mainz, Fed. Rep. of Germany James I. Drever Laramie, WY 82071 Ananda Dube Calcutta 29, India Michael B. Duke Houston, TX 77058 Saeed A. Durrani Birmingham B 15 2TT, U.K. J. Thomas Dutro, Jr. Washington, DC 20560 Thomas C. Duxbury Pasadena, CA 91109 Stephen E. Dwornik Springfield, VA 22151 Palmer Dyal Moffett Field, CA 94035 Robert F. Dymek Cambridge, MA 02138 Daniel Dzuirsin Vancouver, WA 98661 Alexander J. Easton London SW7 5BD, U.K. Dennis D. Eberl* Denver, CO 80225 Peter Eberhardt CH-3012 Bern, Switzerland Burton Edelson Washington, DC 20546 William D. Ehmann Lexington, KY 40506 Henry L. Ehrlich Troy, NY 12108 Farouk E1-Baz Lexington, MA 02173 Charles Elachi Pasadena, CA 91109 Niles Eldridge • New York, NY 10024 Wolf gang Els_on Albuquerque, NM 87131 Peter Englert San Jose, CA 95192-0101 Roy J. Enrico Dallas, TX 75265 Samuel Epstein Pasadena, CA 91125 W. Gary Ernst Los Angeles, CA 90024 Tezer Esat Canberra ACT 2600, Australia Larry W. E,sposito Boulder, CO 80309 O. Eugster 3000 Bern, Switzerland John Evans Richland, WA 99352 Diane L. Evans Pasadena, CA 91109 A. E. Fallick Glasgow, Scotland G75 OQU Fraser P. Fanale Honolulu, HI 96822 Tom G. Farr* Pasadena, CA 91109 Hugo Fechtig* Heidelberg 06221/5161 Mikhail A. Fedonkin* Profsojuznaja ul., 113 William C. Feldman* Los Alamos, NM 87545 Anthony A. Finnerty Davis, CA 95695 APPENDIXB2, con't B2-5

NAME ADDRESS

Edward L. Fireman Cambridge, MA 02138 James Fletcher McLean, VA 22102 Geo. James Flynn Plattsburgh, NY 12901 R. V. Fodor Raleigh, NC 27650 Robert Fogel Providence, RI 02912 Robert O. Fournier Menlo Park, CA 94025 Carl A. Fran,cis Cambridge, MA 02138 P.W. Francis MK7 6AA, England Philip B. Fraundorf St. Louis, MO 63130 Kurt Fredriksson Washington, DC 20560 Bevan French Chevy Chase, MD 20815 Gerald M. Friedman Troy, NY 12180 Louis Friedman Pasadena, CA 91106 E. Imre Friedman Tallahassee, FL 32306 Clifford Frondel Cambridge, MA 02138 Robert Fudali Washington, DC 20560 Takaaki Fukuoka Tokyo 171, Japan M. Fuller Santa Barbara, CA 93106 Michael J. Gaffey • Troy, NY 12180-3590 Edward S. Gaffney Los Alamos, NM 87545 Robert M. Garrels St. Petersburg, FL 33701 James B. Garvin Greenbelt, MD 20771 Donald E. Gaunt Murphys, CA 95247 Johannes Geiss T 3012 Bern, Switzerland E.K. Gibson, Jr.* Houston, TX 77058 R.H. Giese Gab. NB-7, Fed. Republic of Germany Billy P. Glass* Newark, DE 19716 Parmatina S. Goel* Kanpur 208016, India Kenneth A. Goettel Washington, DC 20008 Alexander F.H. Goetz Boulder, CO 80309-0449 Edward D. Goldberg La Jolla, CA 92093 Samuel S. Goldich Golden, CO 80401 Joseph I. Goldstein Bethlehem, PA 18015 Gordon Goles Eugene, OR 97403 Andy M. Gombos. Jr.* Houston, TX 77001 James L. Gooding* Houston, TX 77058 Cyrena Goodrich Tucson, AZ 85721 A. El Goresy Fed. Rep. of Germany J.N. Goswami Ahmedabad, 380009 India Jonathan C. Gradie Honolulu, HI 96822 Monica M. Grady Milton Keynes MK7 6AA, U.K. Andrew Graham London SW7 5BD, U.K. Ronald Greeley* Tempe, AZ 85287 Richard A.F. Grieve Providence, RI 02912 Ralph E. Grim Urbana, IL 61801 Pieter M. Grootes Seattle, Washington 98195 Lawrence Grossman Chicago, IL 60637 Timothy L. Grove* Cambridge, MA 02139 Eberhard Grun Fed. Rep. of Germany J.E. Guest United Kingdom B2-6 APPENDIXB2, con't

NAME ADDRESS

EdwardA. Guinness St Louis, MO 63130 S.Haggerty Amherst, MA 01003 Wendy S. Hale-Erlich New Orleans, LA 70150 Ian Halliday Ottawa, Ontario K IA OR6, Canada Kenneth Hamblin Provo, UT 84602 C.U. Hammer Copenhagen, Denmark Martha Hanner Pasadena, CA 91109 Gilbert N. Hanson Stony Brook, NY 11790 Robert E. Hanss San Antonio, TX 78284 B. Hapke Pittsburgh, PA 15260 Robert B. Hargraves Princeton, NJ 08540 Alan W. Harris Pasadena, CA 91109 Stanley R. Hart Brookline, MA 02146 William K. Hartmann Tucson, AZ 85719 Jack B. Hartung APO New York 09012-5423 Museum of Comparative Zoology Cambridge, MA 02138 Larry A. Haskin St. Louis, MO 63130 B. Ray Hawke Honolulu, HI 96822 J.F. Hays Washington, DC 20550 James W. Head Providence, RI 02912 Grant Heiken Los Alamos, NM 87544 K. F. J. Heinrich Washington, DC 20234 Eleanor F. Helin Pasadena, CA 91109 Karl G. Henize Houston, TX 77058 Donald L. Henninger Houston, TX 77058 Ulrich Herpers D5000 Koln l, Fed. Rep. of Germany Jan Hermeam B-3030 Leuven, Belgium Claude T. Herzberg New Brunswick, NJ 08854 Gregory F. Herzog New Brunswick, NJ 08903 K.G. Heumann Fed. Rep. of Germany Roger H. Hewins New Brunswick, NJ 08903 Richard Hey La Julia, CA 92093 Dieter Heymann Houston, TX 77251 L.J. Hickey Washington, DC 20560 Michael D. Higgins Quebec G7H 2BI, Canada Noel W. Hinners Greenbelt, MD 20771 Peter Hirsch (D-2300) Keil/West Germany JSC Historian Houston, TX 77058 R.D. Hoare Bowling Green, OH 43403 Carroll A. Hodges Menlo Park, CA 94025 Charles M. Hohenberg_ St. Louis, MO 63130 Heindrich D. Holland Cambridge, MA 02138 William T. Holser Eugene, MA 02138 Henry Holt Flagstaff, AZ g6001 Masatake Honda Tokyo 156, Japan Yin Hong-Fu People's Republic of China K. Horai Palisades, NY 10964 Robert J. Horodyski New Orleans, LA 70118 Norman H. Horowitz* La Julia, CA 91125 F. Horz Houston, TX 77058 APPENDIXB2, con't B2-7

NAME ADDRESS

Robert M. Housley Thousand Oaks, CA 91360 Hatten Howard Athens, GA 30602 J. Stephen Huebner Reston, VA 22092 W.F. Huebner Los Alamos, NM 87545 Robert Huguenin Amherst, MA 01003 Glenn I. Huss Denver, CO 80201 Gary R. Huss St. Paul, MN 55108 Ian D. Hutcheon Pasadena, CA 91125 Robt. Hutchison London, S.W. 7, U.K. Donald W. Hyndman Missoula, MT 59812 Yukio Ikeda Mito 310, Japan Andrew P. Ingersoll Pasadena, CA 91125 Trevor R. Ireland Canberra 2601, Australia Anthony J. Irving Seattle, WA 98195 Andrei V. Ivanov Moscow, USSR Marion L. Jackson Madison, Wl 53706 Bruce M. Jakosky Boulder, CO 80309 Odette B. James Reston, VA 22092 Eugene Jarosewich Washington, DC 20560 Raymond Jeanloz Berkeley, CA 94720 J.A. Jeletzky Ottawa, Kls 5B6 Canada E.K. Jessberger Fed. Rep. of Germany William D. Johns Columbia, MO 65211 Torrence V. Johnson Pasadena, CA 91109 Blair F. Jones Reston, VA 22092 Sheldon Judson Princeton, NJ 08540 Anthony J.T. Jull Tucson, AZ 85721 Anne Kahle Pasadena, CA 91109 Ralph Kahn* Washington, DC 20546 Gregory Kallemeyn Los Angeles, CA 90024 I.R. Kaplan Los Angeles, CA 90024 William J. Kaufmann, III Danville, CA 94526 William Kaula Los Angeles, CA 90024 Paul W. Keaton Los Alamos, NM 87544 Klaus Keil Albuquerque, NM 87131 James E. Keith Houston, TX 77058 Walter D. Keller* Columbia, MO 65211 Burton M. Kennedy Berkeley, CA 94720 John E. Kennedy Canada S7N 0W0 John F. Kerridge Los Angeles, CA 90024 Joseph Kerwin Houston, TX 77058 Hugh H. Kieffer Flagstaff, AZ 86001 Makoto Kimura Mita 310, Japan Trude V.V. King Denver, CO 80225 John S. King • Amherst, NY 14226 Elbert A. King Houston, TX 77004 T. Kirsten Fed. Rep. of Germany Margaret Kivelson Los Angeles, CA 90024 Lisa C. Klein Piscataway, NJ 08854 82-8 APPENDIXB2, con't

NAME ADDRESS

Jens Martin Knudsen* DK-2100 Copenhagen, Denmark Michael Kobrick Pasadena, CA 91109 Carl F. Koch Norfolk, VA 23508 R. Craig Kochel Carbondale, IL 62901 Christian Koeberl* A-1010 Wien, Austria Truman P. Kohman Pittsburgh, PA 15213 Paul D. Komar Corvallis, OR 97331 Alan S. Kornac_i Houston, TX 77001 Randy Korotev St. Louis, MO 63130 U. Krahenbuhl CH-3000 Bern 9, Switzerland Konrad B. Krauskopf Stanford, CA 94305 William N. Krebs Denver, CO 80202 David Krinsley Tempe, AZ 85287 Gero Kurat Vienna, Austria A-1014 Ikuo Kushiro Tokyo, 113, Japan Keith Kvenvolden Menlo Park, CA 94025 Philip R. Kyle Socorro, NM 87801 John De Latter Western Australia C. W. Lagle Houston, TX 77058 D. Lal India Chris Lambertsen Philadelphia, PA 19104-6068 Ed Landing Albany, NY 12230 Carl Landuy, dt" Krijgslaan 281, $8, Belgium Bruno Lang 02-089 Warsaw, Poland Yves Langevin Orsay, France Chester C. Langway, Jr. Amherst, NY 14226 John W. Larimer Tempe, AZ 85281 J.C. Laul Richland, WA 99352 Larry Lebofsky . Tucson, AZ 85721 Joshua Lederberg New York, NY 10021 W.P. Leeman Houston, TX 75251 Douglas A. Leich Livermore, CA 94550 Conway B. Leovg Seattle, WA 98195 Gilbert V. Levin Rockville, MD 20852 Eugene H. Levy Tucson, AZ 85721 John S. Lewis Cambridge, MA 02139 Byron J. Lichtenberg Cambridge, MA 02139 Louis Lindner 1009 AJ Amsterdam, Netherland Donald H. Lindsley Stony Brook, NY 11794 David Lindstrom Houston, TX 77058 Marilyn M. Lindstrom Houston, TX 77058 Michael E. Lipschutz W. Lafayette, IN 47907 Gary Lofgre[} Houston, TX 77058 John Longhi- New Haven, CT 06511 Heinz A. Lowenstam Pasadena, CA 91125 Baerbel K. Lucchitta Flagstaff, AZ 86001 Gunter W. Lugmair La Jolla, CA 92093 Maw-Such Ma Melville, NY 11747 J.D. MacDougall La Jolla, CA 92093 APPENDIXB2, con't B2-9

NAME ADDRESS

Glenn J. MacPherson Washington, DC 20560 Ian Mackinnon Albuquerque, NM 87131 Michael C. Malin Tempe, AZ 85287 Rocco Mancinelli* Moffett Field, CA 94305 Oliver K. Manuel Rolla, MO 65401 Kurt Marti* La Jolla, CA 92093 Ursula Marvin Cambridge, MA 02138 Brian H. Mason Washington, DC 20560 Akimasa Masuda Nada, Kobe 657, Japan Harold Masursky Flagstaff, AZ 86001 Dennis Matson Pasadena, CA 91109 Satoshi Matsunami Tokyo 113, Japan D. P. Mattey Cambridge, U.K. Michel Maurette 91406 Orsay, France Ted A. Maxwell Washington, DC 20560 Toshiko Mayeda Chicago, IL 60637 John F. McCauley Flagstaff, AZ 86001 Thomas B. McCord Honolulu, HI 96822 James E. McCoy Houston, TX 77058 Frank B. McDonald Washington, DC 20546 J.A.M. McDonnell Canterbury, Kent, CT2 7NT, U.K. Lucy A. McFadden College Park, MD 20742 James J. McGee Reston, VA 22092 George E. McGill Amherst, MA 01002 Gordon McKay* Houston, TX 77058 Christopher P. McKay Moffett Field, CA 94035 David McKay Houston, TX 77058 Kevin McKeegan St. Louis, MO 63130 Stephen W.S. McKeever Stillwater, OK 74078 Harry Y. McSween, Jr. Knoxville, TN 37916-1410 Charles L. Melcher Ridgefield, CT 06877 H.J. Melosh Tucson, AZ 85721 Wendell W. Mendell Houston, TX 77058 A.E. Metzger Pasadena, CA 91103 Tony Meunier Reston, VA 22092 Henry O.A. Meyer West Lafayette, IN 47907 Charles Meyer • Houston, TX 77058 Michael A. Meyer Tallahassee, FL 32306 Stanley Miller La Jolla, CA 92093 Daniel J. Milton Reston, VA 22092 Douglas W. Ming Houston, TX 77058 David W. Mittlefehldt Houston, TX 77058 Masamichi Miyamoto Tokyo 153, Japan Henry Moore Menlo Park, CA 94025 Carleton B. Moore Tempe, AZ 85287 J.W. Morgan Reston, VA 22092 Richard Morris Houston, TX 77058 Elliott C. Morris Flagstaff, AZ 86001 David Morrison Honolulu, HI 96822 D.A. Morrison Houston, TX 77058 Peter J. Mouginis-Mark Honolulu, HI 96822 B2-10 APPENDIXB2, con't

NAME ADDRESS

W.R. Muehlberger Austin, TX 78712 Duane Muhleman Pasadena, CA 91125 A.B. Mukherjee W. Bengal, India Frederick A. Mumpton Brockport, NY 14420 Bruce Murray Pasadena, CA 91109 M.T. Murrell Pasadena, CA 91125 Charles W. Naeser Denver, CO 80225 Hiroko Nagahara Hongo, Tokyo 113, Japan Hiroshi Nagasawa Tokyo, 171, Japan B. Nagy Tucson, AZ 85721 Andrew F. Nagy Ann Arbor, MI 48102 Noburu Nakamura Nada-ku, Kobe 657, Japan Douglas B. Nash Pasadena, CA 91109 David F. Nava Greenbelt, MD 20771 C.E. Nehru Brooklyn, NY 11210 John M. Neil Sacramento, CA 95825 Joseph A. Nelen Washington, DC 20560 Robert M. Nelson Pasadena, CA 91109 Gerhard Neukum W. Germany H.E. Newsom Albuquerque, NM 87131 Neil Nickle Pasadena, CA 91109 John Niehoff Schaurnberg, IL 60195 Alfred O.C. Nier Minneapolis, MN 55455 Kunihiko Nishiizumi La Jolla, CA 92093 Gordon L. Nord, Jr. Reston, VA 22092 Northrop Services, Inc. Houston, TX 77058 Stewart Nozette Austin, TX 78705 Dag Nummedal Baton Rouge, LA 70803 Joseph A. Nuth Greenbelt, MD 20771 Larry Nyquist Houston, TX 77058 John O'Keefe Greenbelt, MD 20771 Carol O'Neill New York, NY 10024 Edward Olsen Chicago, IL 60605 John Pro Houston, TX 77004 Roll Ostertag West Germany Tobias C. Owen* Stony Brook, NY 11794 Vance I. Oyam_ Moffett Field, CA 94035 David A. Paige Los Angeles, CA 90024 Thomas O. Paine Los Angeles, CA 90024 Herbert Palme Fed. Rep. of Germany Kevin Pang Pasadena, CA 91109 D. A. Papanastassiou Pasadena, CA 91125 J.J. Papike Rapid City, SD 57701 Julie Paque Cambridge, MA 02138 E M Parmentier Providence, RI 02912 Stanton J. Peale Santa Barbara, CA 93106 Paul Pellas Paris 5, France Robert O. Pepin Minneapolis, MN 55455 Gordon Pettengill Cambridge, MA 02139 Roger Phillips Dallas, TX 75275 APPENDIXB2, con't B2-11

NAME ADDRESS

Wm. Phinney Houston, TX 77058 David C. Pieri Pasadena, CA 91109 Carle Pieters Providence, RI 02912 R.J. Pike Menlo Park, CA 94025 C.T. Pillinger* MK7 6AA, Buckinghamshire, U.K. Charles W. Pitrat Amherst, MA 01003 Harry N. Planner Los Alamos, NM 87545 Jeffrey Plescia Flagstaff, AZ 86001 C.W. Poag Woods Hole, MA 02543 James B. Pollack Moffett Field, CA 94035 C.A. Ponnampert_ma College Park, MD 20742 Wayne R. Premo Denver, CO 80225 Frank Press Washingon, DC 20418 P. B. Price Berkeley, CA 94720 Martin Prinz New York, NY 10024 Wm. L. Quaide Washington, DC 20546 R.S. Rajan Pasadena, CA 91109 L. A. Rancitelli Columbus, OH 43201 Kalervo Rankama 00170 Helsinki 17, Finland M.N. Rao Ahmedabed-380 009, India A.S.P. Rao Hyderabad-500 007, India U.R. Rao Bangalore-560 009, India Kaare L. Rasmussen 2200 Copenhagen, Denmark David M. Raup Chicago, IL 60605 D.G. Rea Pasadena, CA 91109 S. J. B. Reed Cambridge CB2 3EW, U.K. George W. Reed, Jr. Argonne, IL 60439 Robert C. Reedy* Los Alamos, NM 87545 Arch M. Reid Houston, TX 77004 Wolf Uwe Reimold Johannesburg 2000, South Africa John H. Reynolds Berkeley, CA 94720 J.M. Rhodes Amherst, MA 01003 Steven M. Richardson Ames, IA 50011 Frans J.M. Rietmeyer* Albuquerque, NM 87131 J. Keith Rigby Provo, UT 84602 A. E. Ringwood Canberra, ACT 2600, Australia R.F. Rissone Swinton, SN2 lET, England Barrett N. Rock Pasadena, CA 91109 David J. Roddy Flagstaff, AZ 86001 Edwin Roedder Reston, VA 22092 Jeff Rosendahl Washington, DC 20546 Lisa Rossbacher Pomona, CA 91768 George R. Rossman Pasadena, CA 91125 Ladislav Roth Pasadena, CA 91109 Marvin W. Rowe College Station, TX 77843 A. Ru Rozanov Profsojuznaja ul., 113 Alan Edward Rubin Los Angeles, CA 90024 Marvin L. Rudee La Jolla, CA 92037 Keith Runcorn United Kingdom NEI 7RU C.T. Russell Los Angeles, CA 90024 Pat Russell Washington, DC 20001 B2-12 APPENDIXB2, con't

NAME ADDRESS

GrahamRyder Houston, TX 77058 CarlSagan Ithaca, NY 14853 JackSalisbury Reston, VA 22092 Frank B. Salisbury Logan, UT 84322-4820 Peter Salpas Auburn, AL 36849-3501 Scott Sandford _ Moffett Field, CA 94035 M. Sato Reston, VA 22092 R.S. Saunders Pasadena, CA 91103 Norman M. Savage Eugene, OR 97403 Samuel M. Savin Cleveland, OH 44106 Gerald Schaber Flagstaff, AZ 86001 Roman A. Schmitt Corvallis, OR 97331 Harrison H. Schmitt Albuquerque, NM 87191-4338 Charles Schnetzler Greenbelt, MD 20771 J. William Schopf Los Angeles, CA 90024 Henry D. Schreiber Lexington, VA 24450 Gerald Schubert Los Angeles, CA 90024 Peter Schultz Providence, RI 02912 Ludolf Schultz Fed. Rep. of Germany Henry P. Schwarcz Canada L8S 4MI Ronald F. Scott Pasadena, CA 91125 Edward R.D. Scott Albuquerque, NM 87131 David H. Scott Flagstaff, AZ 86001 Derek W. Sears Fayetteville, AR 72701 Tom See Houston, TX 77058 J.J. Sepkoski Chicago, IL 60637 Mark Settle Piano, TX 75075 Robert P. Sharp Pasadena, CA 91125 D. M. Shaw Hamilton, Ontario, Canada LSS 4MI Michael F. Sheridan Tempe, AZ 85287 Masato Shima Tokyo 110, Japan Makoto Shima Yokohama, Japan T240 Eugene M. Shoemaker Flagstaff, AZ 86001 Nicholas Short Greenbelt, MD 20771 Richard Shorthill Salt Lake City, UT 84112 Peter Signer Zurich, Switzerland Godfrey Sill Tucson, AZ 85721 Leon T. Silver Pasadena, CA 91125 Tom Simkin Washington, DC 20560 Steven Simon Rapid City, SD 57701 Patrica A. Sims* SW7 5BD, England Robert Singer Tucson, AZ 85721 C.S.P. Singh Varanasi 221005, India Brian J. Skinner New Haven, CT 06520 Monty R. Smith Richland, WA 99352 Brad Smith Tucson, AZ 85721 Joseph V. Smith* Chicago, IL 60637 Roger S. U. Smith Austin, TX 78712 Roman Smoluchowski Austin, TX 78712 Joseph R. Smyth Boulder, CO 80309-0250 APPENDIXB2, con't B2-13

NAME ADDRESS

JohnSnyder Washington, DC 20550 Larry A. Soderblom Flagstaff, AZ 86001 SeanC. Solomon Cambridge, MA 02139 C.P.Sonett Tucson, AZ 85721 FrankJ. Spera Santa Barbara, CA 93106 Cary R. Spitzer Hampton, VA 23665 JohnSplettstoesser St. Paul, MN 55114 PaulD. Spudis Flagstaff, AZ 86001 StevenW. Squyres Moffett Field, CA 94035 G.M. Stanley, Jr. Washington, DC 20560 Ian M. Steele Chicago, IL 60637 James B. Stephens Pasadena, CA 91109 James H. StiLt Columbia, MO 65211 Carol Stoker Moffett Field, CA 94307 Edward D. Stolper Pasadena, CA 91125 Charles D. Stone Austin, TX 78713 G. Stotzky New York, NY 10003 Patricia A. Straat Rockville, MD 20852 Melissa Strait Alma, MI 48801 David W. Strangway Vancouver, B.C., Canada V6T 2B3 Ed Strickland Leander, TX 78722 Robert G. Strom Tucson, AZ 85721 Hans Suess San Diego, CA 92037 David E. Sugden Aberdeen AB9 24F, Scotland Naoji Sugiura Ontario, Canada L5L 1C6 Robert M. Sullivan Boulder, CO 80309 Kathryn D. Sullivan Houston, TX 77058 Steve Sutton Upton, NY 11973 Gordon A. Swarm Flagstaff, AZ 86001 Peter Swart Miami, FL 33149 Walter C. Sweet Columbus, OH 432 l0 Nobuo Takaoka Yamagoto, 990, Japan Hiroshi Takeda Hongo, Tokyo 113, Japan Kim H. Tan* Athens, GA 30602 Ken Tanaka* Flagstaff, AZ 86001 Tsuyoshi Tanaka Ibaraki, 305 Japan Helen Tappan Los Angeles, CA 90024 James Taranik Washington, DC 20546 Mitsunobu Tatsumoto* Denver, CO 80225 G. Jeffrey Taylor Albuquerque, NM 87131 S.R. Taylor Canberra, Australia Lawrence A. Taylor Knoxville, TN 37996 Klaus Thiel Fed. Rep. of Germany Mark H. Thiemens* La Jolla, CA 92093 H.G. Thode Hamilton 16, Ontario, Canada David E. Thompson Washington, DC 20546 Lonnie G. Thompson* Columbus, OH 43210 Theodore W. Tibbitts Madison, WI 53706 Allen Tice Hanover, NH 03755 Shelby Tilford Washington, DC 20546 Robert Tilling Reston, VA 22092 B2-14 APPENDIXB2, con't

NAME ADDRESS

G.R.Tilton Santa Barbara, CA 93106 M. Nafi Toksoz Cambridge, MA 02139 T.A. Tombrello Pasadena, CA 91109 KazushigeTomeoka Tempe, AZ 85287 OwenBrian Toon Moffett Field, CA 94035 PriestlyToulmin, III Reston, VA 22301 KennethM. Towe Washington, DC 20560 Allan H. Treiman* Boston, MA 02215 JacobI. Trombka Greenbelt, MD 20771 Akira Tsuchiyama Kyoto 606, Japan Karl K. Turekian New Haven, CT 06511 AnthonyTurkevich Chicago, IL 60637 G. Turner Sheffield $3 7RH, U.K. F.C.Ugolini Seattle, WA 98195 D.R. Uhlmann Cambridge, MA 02139 JamesR. Underwood,Jr. Manhattan, KS 66506 W.R.Van Schmus Lawrence, KS 60044 David Vaniman Los Alamos, NM 87545 MichaelAnthonyVelbel* East Lansing, MI 48824 GeeratJ. Vermeij College Park, MD 20742 JosephVeverka Ithaca, NY 14853 Faith Vil_s Houston, TX 77058 R.D. Vis-- Amsterdam 1007MC, The Netherlands Alex Volborth Butte, Montana 59701 Tyler Volk New York, NY 10003 W. VonEngelhardt Tuebingen, Fed. Rep. of Germany John F. Wacker La Jolla, CA 92093 Robert M. Walker St. Louis, MO 63130 Dave Walker* Palisades, NY 10964 Steven D. Wall Pasadena, CA 91109 Heinrich Wanke 6500 Mainz, Fed. Rep. of Germany Stanley H. Ward Salt Lake City, UT 84112 A. Wesley Ward Flagstaff, AZ 86001 Bruce R. Wardlaw Denver, CO 80225 David Wark Tucson, AZ 85721 Jeffrey L. Warner* La Habra, CA 90631 Paul H. Warren Los Angeles, CA 90024 G.J. Wasserburg Pasadena, CA 91125 John Wasson Los Angeles, CA 90024 P.W. Weiblen Minneapolis, MN 55455 D.F. Weill Eugene, OR 97403 Michael K. Weisberg New York, NY 10024 Paul R. Weissmann Pasadena, CA 91109 David B. Wenner Athens, GA 30602 G.W. Wetherill Washington, DC 20015 W. Brian Whalley Northern Ireland, UK Ian Whillans Columbus, Ohio 43210 Fred L. Whipple Cambridge, MA 02138 David C. White Tallahassee, FL 32306 I.P. Wright* Buckinghamshire, UK J.L. Whitford-Stark Alpine, TX 79832 APPENDIXB2, con't B2-15

NAME ADDRESS

Don E. Wilhelms Menlo Park, CA 94025 Laurel L. Wilkening Tucson, AZ 85721 Richard Williams Houston, TX 77058 John L. Williams Denver, CO 80202 John Willis Bethlehem, PA 18015 M.V.H. Wilson T6G 2E9 Canada S.L. Wing Menlo Park, CA 94025 Donald Wise Amherst, MA 01002 S.W. Wise Tallahassee, FL 32306 Frank Wlotzka D-65 Mainz, Fed. Rep. of Germany Charles A. Wood Houston, TX 77058 John A. Wood Cambridge, MA 02138 Joe Wooden Menlo Park, CA 94025 Dorothy S. Woolum Fullerton, CA 92634 Alexander Woronow Houston, TX 77004 Thomas L. Wright Hawaii Natl. Park, HI 96718 Ian Wright Buckinghamshire, UK Sherman S.C. Wu Flagstaff, AZ 86001 Peter Wyllie Pasadena, CA 91125 Crayton J. Yapp Albuquerque, NM 87131 Ellis L. Yochelson Washington, DC 20560 Hatten S. Yoder, Jr. Washington, DC 20008 Ed Zeller Lawrence, KS 66045 Benjamin H. Zellner Tuscon, AZ 85721 Aaron P. Zent* Honolulu, HI 96822 Herman Zimmerman Washington, DC 20550 E. Zinner St. Louis, MO 63130 William Zinsmeister Columbus, OH 43210 Mike Zolensky Houston, TX 77058 Herbert Zook Houston, TX 77058 Jack Zussman Manchester M l3 NPL UK

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• _ "_ _ .* I_J/l_/I REPORT DOCUMENTATION PAGE Natfonal Aeronautics and S_ce Administration

1. Report No. 2. Government Accession No. 3. Reciplent's Catalog No. NASA TM-41_4

4. Title and Subtitle 5. Repor¢ Date

Scientific Guidelines for Preservation of Samples Collected Aprll 1990 From Mars 6. Performing Organization Code SN21 7. Author(s) 8. Performmg Organization Report No. James L. Gooding, Editor 5-604

9. Performing Organization Name and Address 10, Work Unit NO.

Planetary Science Branch 11. Contract or Grant No. NASA/Johnson Space Center Houston_ TX 77058 12. Spon_ring Agency Name and Address 13. Type of Report and Period Covered

Solar System Exploration Division Techni ca1 Memorandum NASA/Johnson Space Center 14. Sponsoring Agency Code Houston, TX 77058

15. Supplementary Notes

16. Abstract

The maximum scientific value of Martian geologic and atmospheric samples is retained when the samples are preserved in the conditions that applied prior to their collection. Any sample degradation equates to loss of information. Based on detailed review of pertinent scientific literature, and advice from experts in planetary sample analysis, number values are recommended for key parameters in the environmental control of collected samples _ith respect to material contamination, temperature, head-space gas pressure, ionizing radiation, magnetic fields, and acceleration/shock. Parametric values recommended for the most sensitive geologic samples should also be adequate to preserve any biogenic compounds or exobiological relics.

7. Key Words (Suggested by Author(s)) 18. Distribut,on Statement

Mars, Sample preservation Unclassified- Unlimited Subject Category 91

19. Secunty CIasslficat=on (of this report) J 20. Security Classdication (of this page) I 21. NO. of pages I 22. Price APPENDIX B3 B3-111

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APPENDIX B4

ESTIMATES OF MARTIAN "OXIDANT" ABUNDANCES IN SEDIMENT SAMPLES AT THE VIKING LANDING SITES

James L. Gooding

SN21/Planetary Science Branch, NASA/Johnson Space Center, Houston, TX 77058.

Introduction. The life-detection experiments on the Viking Landers obtained apparently positive responses which, after initial evaluation as possible biological activity, were inferred to be signatures of highly reactive inorganic chemical agents in the Martian sediment samples. As reviewed by Klein [1], the complete set of results indicated that at least two (and possibly three or more) different agents occurred in the samples. Given the fundamentally different nature of the three biology experiments and their results, it was concluded that, at the minimum, the set of reactive agents possessed the capacities to evolve molecular oxygen by reaction with water, to oxidize simple organic compounds in aqueous solution, and to fix gaseous carbon dioxide into forms that are non-volatile under nominal Martian surface conditions. Despite those very different properties, the oxidization reactions received more popular attention and the reactive agents became known collectively as "oxidants _. Although the experiment teams explored various explanations for the Viking results, derived values for the abundances of the "oxidants" were apparently never published. The simple calculations presented here purport to use the Viking measurements to estimate the concentrations of reactive agents in the original sediment samples. Such estimates are needed both to support preservation plans for returned Martian samples and to assist in design of future Mars surface experiments. As will be shown, there is no single, preferred concentration value. Instead, it is found that the "oxidant" concentrations were probably in the range of a few parts per billion (ppb) to a few hundred parts per million (ppm) by weight.

Data and Assumptions. Upper limits for abundances of the reactants can be estimated from the most active samples (i.e., those giving the greatest "positive" results) in the Viking Lander gas-exchange (GEX), labelled release (LR) and carbon assimilation (CA; also known as pyrolytic release, PR) experiments. Other samples showed less activity, presumably because they contained lower abundances of the active chemical agents. Data used here are those reported by the original investigator teams [2-5]. Assuming a bulk density of 1.5 g/cm 3 for the delivered soil samples of specified volume, the masses of the samples analyzed were approximately 1.5 g (GEX), 0.75 g (LR), and 0.38 g (CA/PR), respectively. For simplicity, instrument-based differences between actual decay rates and measured count rates are ignored here for LR and CA/PR. Most interpreters of the Viking biology results have favored one or more metal peroxides or superoxides as the active agents for the observed phenomena. Because computational results of the type presented below depend on the molecular weight (hence, identity) assumed for the oxidant and the stoichiometry assumed for the pertinent reactions, caution must be exercised in interpreting the derived numbers; they are intended to represent only the order-of-magnitude concentrations of the compounds in question. For simplicity, the following results assume the stoichiometry appropriate for alkali-metal peroxides (M20 2) as model reactants and express results in equivalent concentrations of H20 2. It should not be inferred, however, that this procedure represents an endorsement of H202 as the active agent in any of the Viking biology experiments. Alternative models, based on catalytic properties of clay minerals [6,7] deserve separate attention and are not treated here.

Results for GEX. The GEX, VL-1 "Sandy Flats" (first cycle, humid) sample released 790 umol 0 2 after wetting of 1 cm 3 of soil with 0.56 em 3 of aqueous nutrients [5]. If evolution of 0 2 was an inorganic process, for which the organic nutrients were simply spectators in a water/peroxide reaction, each mole of 0 2 produced would require consumption of two moles of peroxide: 2

M20 2 + H20--> 1/2 0 2 + 2MOH.

Therefore, the abundance of peroxide would be 2(7.9 x 10.7 mol)/1.5 g = 1.05 x 10-6 mol/g sample. If the peroxide was H20 2 (f.w. 34.0), the implied abundance would be

(1.05 x 10-6)(34.0) = 36 ppm.

Using laboratory simulations with photo-oxidized MnO 2 to duplicate the GEX results, Blackburn et al. [8] pointed out that 790 nmol of O 2 could be produced by only 1.9 x 1018 atoms of activated Mn. That amount would correspond to only 1.2 x 10-4 g Mn/g sample, or only 120 ppm Mn in the sample. If the oxidant was MnO3H (f.w. 103.9), as suggested by Blackburn et al. [8], then its equivalent concentration would have been (1.2 x 10-4)(103.9/54.9) = 230 ppm.

Results for LR. The LR, VL-2, under "Notch Rock" (third cycle) sample produced 15,500 dpm of 14C after injection of 0.115 cm 3 of aqueous nutrient onto 0.5 cm 3 of sample [3]. The nutrient consisted of 7 organic compounds, each at a concentration of 2.5 x 10-4 M and with an average labelled activity of 8 # Ci//_ mol [2]. The carbon gas evolved (presumably CO2) contained at the minimum the number of carbon atoms equivalent to the measured radioactivity. Most likely (but not substantiated by the experiment), the evolved gas also contained non-radioactive carbon in the same proportion as the 14C/(total C) ratio in the original nutrients. Therefore, at least two different estimates for oxidant abundance are possible. The number of 14C atoms should be related to the decay rate according to N = (1/)_)(dN/dt), where A = 1.21 x 10 -4 y-1 = 2.30 x 10-1° m -1. Therefore, using the measured activity, the minimum (all 14C) "efficiency" of carbon consumption was [(1.55 x lif t m-1)/(2.30 x 10-10 m'1)]/[(6.02 x 1023 mo1-1)(0.75 g)] = 1.49 x 10-10 mol C/g sample. A second, higher estimate could be made by assuming that the specific activity (on a molar basis) of the evolved gas was not changed by the oxidation reaction(s). (The most plausible change, but one not addressed by the experiment, would have been mass-dependent fractionation of the carbon isotopes by oxidation). The assumption of constant specific activity in the nutrients and the evolved gas permits a gas yield of [(1.55 x 104 m-l)(1 m/60 s)]/[8 Ci/mol)(3.7 x 1010 s-1/Ci)(0.75 g)] = 1.16 x 10-9 mol C/g sample. If the oxidation reaction involved a 1:1 molecular ratio of oxidant to nutrient (e.g., M202/HCOONa ), then the decarboxylation "efficiency" number also corresponds to the moles of oxidant per gram of sample. Reducing the yields to a basis of H20 2 concentrations, as done above for GEX, gives the following two estimated concentrations:

(1.49 x 10-1°)(34.0) = 5.1 ppb (1.16 x 109)(34.0) = 39 ppb.

A third estimate can be made by accepting the interpretation [1,2] that the equivalent of one 14C- labelled nutrient was quantitatively oxidized by the most reactive sample. (Although partial oxidation of several different nutrients cannot be excluded by available data, quantitative consumption of the formate nutrient became the favored interpretation, because of the model simplicity offered by a one-carbon compound). Given the concentration and volume of each LR inoculation, the absolute quantity of each nutrient in the subject experiment was (2.5 x 10-4 mol/103 cm3)(0.115 cm 3) = 2.9 x 10,8 tool. Assuming the same 1:1 stoichiometry for oxidation used above and an H20 2 basis, the alternative estimate for the "oxidant" concentration would be

(2.9 x 10-8)(34.0)/(0.75) = 1.3 ppm.

Results for CA/PR. The CA/PR, VL-1, "Sandy Flats N (C1) sample produced 842 dpm of 14C (corrected Peak 2) after incubation of 0.25 cm 3 of sample [4] with 20 # l of 14C-labelled CO 2 and CO (98:2 by volume; total activity of 22 # Ci) in a 4 cm 3 test cell filled with Martian atmosphere (95% CO2) at 7.6 mb pressure and a temperature of 17° C [2]. The 14C spike increased the total cell pressure by 2.2 mb [2]. ByanalogywithLR, the simplest minimum estimate for the carbon actually t'Lxed can be found from the number of 14C atoms that were fixed. Following the first-order decay method used for LR, the minimum "efficiency" for carbon fkation in CA/PR was [(8.42 x 102 m-1)/(2.30 x 10-10 m'1)]/[(6.02 x 1023 mo1-1)(0.38 g)] -- 1.60 x 10-11 tool C/g sample. Again, by analogy with LR (and ignoring possible mass- dependent fractionation of carbon during reaction), an alternative estimate can be made by assuming no change in specific molar activity during carbon fixation (i.e., Martian CO 2 was fbced along with the labelled CO_2). For ideal gas behavior, the total activity per mole of CO_ in the cell before reaction would be (2.2 x 10-_ Ci)/[((7.6 + 2.2)/1013 atm)(4 x 10-3 1)(0.95)/(8.21 x 10-L 1 atm Kd mo1-1)(290 K)I = 1.42 x 101 Ci/mol. From the measured 14C activity in the fixed carbon, the "efficiency" of fixation would follow as [(8.42 x 102 m'l)(1 m/60 s)]/[(1.42 x 101 Ci/mol)(3.7 x 101° sd/Ci)(0.38 g)] = 7.03 x 10-11 mol C/g sample. The experiment team originally suggested [2] a conversion factor of (2.6 x 10-11 mol CO2/81 dpm) = 3.2 x 10-13 mol C/m -1 14C which, by the reasoning presented here, would have led to a fixation "efficiency" of (3.2 x 10"13)(8.42 x 102)/(0.38) = 7.09 x 10-10 mol C/g sample. On an H202-equivalent basis, the consequent estimates for f'txation-reactant concentration according to these three different model assumptions would be

(1.60 x 10-11)(34.0) = 0.54 ppb (7.03 x 10-11)(34.0) = 2.4 ppb (7.09 x 10-10)(34.0) = 24 ppb.

An additional complication exists in CA/PR because CO is not distinguished from CO 2 among the reactants and products [2,4]. Because the 14CO2 in the experimental gas spike possessed a lower specific activity than the 14CO, the three estimates given immediately above could actually be lower (by as much as a factor of 3) if CO was a major reaction participant [4]. It is important to note that, as originally pointed out by the experiment team [2,4], the active agent detected by the CA/PR experiment might not be an "oxidant". In principle, either an oxidizing or reducing agent (or a third category, "organic-synthetic catalyst") might have produced the carbon fixation.

Summary and Conclusions, The simplest interpretations (i.e., those with the fewest model assumptions) of the three Viking biology experiments imply abundances for the unidentified oxidants/reactants comprising 36 ppm (GEX), 5 ppb (LR), and 0.5 ppb (CA/PR), when expressed in equivalent concentrations of H20 2. The LR and CA/PR results, in particular, are open to a wide range of model assumptions that can support other H202-equivalent concentrations up to 24 ppb (CA/PR) or 1 ppm (LR). The values so derived are fundamentally uncertain because both the molecular weights of the reactants and the stoichiometry of the subject reactions remain unknown. The important point is not the specific number values but the fact that the chemical agents responsible for the Viking biology results occurred at exceedingly small concentrations. Even if several different oxidants/reactants were involved, they would require either very high molecular weights (at least 10 times that of H202) or disproportionately large reaction coefficients (i.e., high reactant/evolved-gas ratio) in order for their total concentrations to exceed a few hundred ppm by weight in the samples. The trace levels of the "oxidants" must be appreciated both for Mars sample-return missions and for design of future in situ Mars sample analyzers. It will be scientifically important to carefully preserve at least some subset of samples in a way that maximizes the opportunity to study these rare, metastable compounds in the laboratory; their low abundances will mean that they may be difficult to isolate for identification. Any experiments proposed to identify the "oxidants" in situ must be able to perform diagnostic analyses of analytes that occur at the ppb to ppm levels. References

[1] Klein H. P. (1978) The Viking biological experiments on Mars. Icarus, 34, 666-674.

[2] Klein H. P., Horowitz N. H., Levin G. V., Oyama, V. I., Lederberg J., Rich A., Hubbard J. S., Hobby G. L., Straat P. A., Berdahl B. J., Carle G. C., Brown F. S., and Johnson R. D. (1976) The Viking biological investigation: preliminary results. Science, 194, 99-105.

[31 Levin G. V. and Straat P. A. (1976) Viking labelled release biology experiment: interim results. Science, 194, 1322-1329.

141 Horowitz N. H., Hobby G. L., and Hubbard G. S. (1977) Viking on Mars: the carbon assimilation experiment. J. Geophys. Res., 82, 4659-4662.

[51 Oyama V. I. and Berdahl B. J. (1977) The Viking gas exchange experiment results from Chryse and Utopia surface samples. J. Geophys. Res., 82, 4669-4676.

[61 Banin A. and Margulies L. (1983) Simulation of Viking biology experiments suggest smectites not palagonites as martian soil analogues. Nature, 305, 523-525.

[71 Burt D. M. (1989) Iron-rich clay minerals on Mars: Potential sources or sinks for hydrogen and indicators of hydrogen loss over time. Proc. 19th Lunar Planet. Sci. Conf., 423-432.

[81 Blackburn T. R., Holland H. D., and Ceasar G. P. (1979) Viking gas exchange reaction: simulation on UV-irradiated manganese dioxide substrate. J. Geophys. Res., 84, 8391-8394.

I%l_t._l/%rlln_ REPORT DOCUMENTATION PAGE National Aeronautics and Space Administration

1. Report NO. 2. Government Accession NO. 3. Reciplent's Catalog No.

NASA TH-4184

4. Title and Subtitle S. Report Date

Scientific Guidelines for Preservation of Samples Collected April 1990 From Mars 6. Performing Organization Code SN21 7. Author(s)

James L. Gooding, Editor 8. Performing Organization Report No. S-604

9. Performing Organization Name and Address 10. Work Umt NO.

Planetary Science Branch 11. Contract or Grant No. NASA/Johnson Space Center Houston I TX 77058 12. Sponsoring Agency Name and Addre_ 13. Type of Report and Period Covered Solar System Exploration Division Technical Memorandum NASA/Johnson Space Center Houston, TX 77058 14. SponsOring Agency Code

15. Supplementary Notes

16. Abstract

The maximum scientific value of Martian geologic and atmospheric samples is retained when the samples are preserved in the conditions that applied prior to their collection. Any sample degradation equates to loss of information. Based on detailed review of pertinent scientific literature, and advice from experts in planetary sample analysis, number values are recommended for key parameters in the environmental control of collected samples _ith respect to material contamination, temperature, head-space gas pressure, ionizing radiation, magnetic fields, and acceleration/shock. Parametric values recommended for the most sensitive geologic samples should also be adequate to preserve any biogenic compounds or exobiological relics.

17. Key Words (Sugge_ed by Author(s)) 18. Distribution Statement

Mars, Sample preservation Unclassified- Unlimited Subject Category 91

19. Security Classdicat_on (of this report) 20. Securi_ Clarification (of this page) 21. No. of pages 22. Price All Unclassified Unclassified 242

For sale by the Nat=onal Techmcal Informat=on Serwce, SprFngfield, VA 22161-2171

NASA-Langley, 1990