master thesis.c-2

UNIVERSITY OF COPENHAGENFaculty of Science

MASTER THESIS

Mars Environmental Chamber for Simulation ofWeathering Processes on Mars

NEW_JMMC

Author: Rita Edit Kajtár Supervisors: Morten Bo MadsenAsmus Koefoed

February the 3rd, 2014

I dedicate this thesis to my parents and grandparents,thanking them for their love and endless support.

AbstractThe present thesis describes the experimental work carried on with the aim of obtaining

the masters degree in physics at the Niels Bohr Institute, University of Copenhagen. Thepurpose of an experimental work done in preparation of the thesis was the establishment ofa New Environmental Chamber, thus creating a facility where various phenomena observedor speculated to occur on the planet Mars can be simulated and studied under realistic (andenhanced) Mars surface environmental conditions. The NEW_Jens Martin Mars Chamber(NEW_JMMC) includes a Quadrupole Mass Spectrometer and pressure transducer, whichmakes it now possible to control a simulated environment similar to Martian conditionsinside the reaction chamber, with relatively high precision.

The actual environmental chamber is itself sheltered from a variable Earth laboratoryenvironment by being placed inside a glovebox which represents a very practical add-onto the original set-up. The glove box is a sealed container, where an inert atmospherecan be introduced and controlled with the purpose of preventing contamination duringexperiments. It also enables sample exchange between different sealed containers, whichcan be later moved elsewhere for analysis.

When assembly, tests and calibration of instruments in the chamber completed, anexperiment focusing on the study of the weathering products resulting from strongUV-exposure of pure surfaces of the mineral olivine was conducted. Finally, the exposedsurfaces and two sets of witness samples were examined by SEM analysis in order tocheck a hyphothesis that the mineral olivine may contribute to the formation ofnanophase oxides present in the reddish Martian dust.

Dansk resuméDenne afhandling beskriver et eksperimentelt arbejdet, der er blevet udført for at

etablere en ny facilitet dedikeret til studier i et realistisk Mars-lignende miliø, hvorforskellige fænomener kan styres med høj præcision. Det opbyggede miljø-kammerNEW_JMMC er blevet udstyret med et indbygget Quadrupole Masse Spektrometer ogtryktransducer, sådan at de simulerede Mars betingelser i reaktionskammeret kan styresmed høj præcision.

Miljøkammeret ligger beskyttet i en handske-boks hvilket er en meget praktisk tilføjelsetil opstillingen. Handskeboksen er en forseglet beholder, hvor vacuum-kammeret befindersig - og hvor der kan etableres en inert atmosfære, der forhindrer forurening under forsøgeneog giver også mulighed for udveksling af prøver mellem forskellige lukkede beholdere, somsenere kan flyttes til analyse andetsteds. Da samleprocessen og kalibreringer var blevetafsluttet, blev et eksperiment udført for at studere produkter fra forvitring af olivin. Olivinhar været eksponeret for ultraviolet stråling og carbondioxid-atmosfære. Endelig, blev deeksponerede overflader undersøgt med SEM analyse for at checke nanofase oxider.

CoverThe cover image represents the front view of the NEW_JMMC sheltered by the glove

box. The picture was taken by Asmus Koefoed and later edited by the author.

Acknowledgements

The assembly of the NEW_JensMartinMarsChamber would not have been possiblewithout a constant collaboration with a part of the academic staff of the Niels BohrInstitute and workshop engineers and without the unconditional support andunderstanding of family and friends. I would like to thank to all those who helped meduring the working process and who very kindly and professionally have assisted me:Asmus Koefoed and Morten Bo Madsen for their constant guidance and extremely fastfeedback, Carsten Mortensen (and the entire team from the mechanical workshop) andAxel Boisen from the electrical workshop, for their incredible work and infinite patience,Nader Payami, Matthew S. Johnson, Claus Sørensen, Jonathan P. Merrison (ÅrhusUniversity) for always giving important advice and suggestions, to Klaus Bechgaard andBo W. Laursen (Chemistry Dept.) for borrowing the glovebox, to Jonas Olsson forhelping to coat and analyze the olivine samples, Magnus Torvald Joelsson for helping totake the UV spectrum of the Xe arc lamp, to Jannis Bouchikas and Jess Martin(Quantum Devices Dept.) for providing additional help throughout my work and also tothe Danish Council for Independent Research/Natural Sciences (FNU grants 12-127126and 11-107019) and to the TICRA Foundation for funding the purchases of equipmentfor the chamber. Further on, I would like to thank to my mother, my father and mygrandparents, to Alexandra and my entire family who have always supported andbelieved in me, to all my friends and especially to Alex, who made everything mucheasier by always being there.

Preface

Motivation for the selected topic

During the first year of my Master studies at the Faculty of Science, I had theopportunity to wander among different fields of study, from Geophysics to Astrophysics,evaluating individually each one of them and sorting out the ones which I really had aninterest for. First, I had a strong inclination towards subjects related to Ice and Climatebut very soon I discovered more attractive ones which made me reconsider my optionsfor the topic of my Master Thesis. The Astrophysics courses have been more interestingand fascinating for me, thus I decided to choose a topic from this field.

Choosing my thesis supervisor was probably the easiest task of the entire process, whilethe subject of my paper came as a result of a debate where both of us have proposed afew ideas to take into consideration and finally were able to deliberate.

In 2011, the first version of the Jens Martin Mars Chamber was made by AsmusKoefoed within the Mars Group at the Niels Bohr Institute. This chamber was aprototype able to provide relatively fair conditions for simulating some of theenvironmental parameters present on Mars, in order to determine how the mineralolivine weathers in such an environment and what happens afterwards. By the time, thiswork has brought many answers; however, it left room for a second try in the attempt ofgetting more precise results while trying to overcome most of the early limitationsencountered at the construction of the chamber.

I was more than happy to accept the challenge of rebuilding the JMMChamber andto try to bring significant improvements in terms of design and functionalities. Both theconstruction of the necessary experiment equipment itself and the challenge of making asustainable environment where an experiment could be conducted, made me aware of theimportance of the work I was about to start.

By signing up for this project, my tasks started to take shape in terms of gaining thenecessary insight into disciplines such as vacuum equipment engineering, electronics,geology, chemistry, mass spectroscopy and scanning electron microscopy and combiningthem, to set-up a relevant experiment. The multidisiplinarity itself implied by theproject is wide and complex.

Work background, objective and limitations

The idea of creating a Mars Environmental Chamber appeared within the Mars Groupat the Niels Bohr Institute as an experimental exercise. The purpose was to create arelatively complex system where further experiments reproducing phenomena observed onMars to be conducted. By building it up and gaining a relatively high approach to theMartian conditions, different investigations became possible to be carried out.

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The possibility to create nanophase iron oxides on the surface of freshly cleaved olivinewas also analyzed.

The first attempt in this direction was made by Asmus Koefoed almost three years ago,whose mission became a demanding one; fortunately, the amount of ideas and strategiesthat led to a well conducted experiment was a constant driving force, sufficient enough toovercome the lack of funding for the project at the time; however, this funding insufficiencycaused a significant delay for the entire project.

The name given to the chamber right at the beginning of its creation, JMMC whichstands for Jens Martin Martian Chamber, was given in the honor of the Danishastrophysicist Jens Martin Knudsen who has left a strong mark in the Danish andinternational Mars exploration. For obvious reasons, the new version of the chamberbecame NEW_JMMC.

The second attempt in creating the NEW_JMMC, an improved version of the chamber,turned out to be my responsibility, having Asmus’s paper as a very important guidingsupport throughout both my theoretical and experimental work.

The objective of my work became to reassemble the Martian environmental chamberfrom scratch, by using some of the spare parts that made up the old chamber but alsousing new and improved equipment components. The adopted work strategy was astraightforward one, meaning that I considered the Future Developments section fromAsmus’s Master thesis to be the list of my future tasks.

Although most of these suggested developments have been met throughout my work,other limitations appeared along the way. Due to the multidisciplinarity of thetheoretical background implied in the thesis, colaboration with workshop manufacturersand unpredicted delay in delivery of ordered components, mostly the time constraintslimited some of the supporting arguments to be further developed.

Structure of the thesis

Throughout the reading of this thesis, one will find it structured in four main parts,where each of them is individualized by the type of research systematically done duringthe study process.

The first chapter has a focus on describing the theoretical background of the paper,including a review of the supporting literature. Relevant articles and materials werestudied in order to be able to extract the majorly accepted idea behind the nano phaseiron oxides formation in the Martian regolith and a few examples of other MarsEnvrionmental Chambers around the world, were given.

The second chapter briefly describes the supporting theory of quadrupole massspectrometry and the technical information of our quadrupole mass spectrometer. Adeeper insight into what is happening when a gas analysis is going on was gained, andthe chapters presenting the scientifc data about the UV radiation flux, average pressureand temperature at the surface of Mars were completed with the developments done inorder to have these parameters simulated in the NEW_JMMC.

Although old dated articles or books provided a trustful source of information, themost recent studies and achievements have been chased along the documentation sessions.The study and discovery of Mars are real time ongoing processes, therefore the informationwe know may be outdated within very short periods of time.

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The third chapter comprises exclusively the methodology and the experimental workdone at the NEW_JMMC. It contains the part where the assembly of the chamber itselfhas been described, pointing out the functionality and the key features of each individualbuilding part. Operating procedures and calculation of the chamber volume are alsodescribed in this chapter. Hazards that are likely to occur at the workplace and safetymeasures are pointed out as well.

The last chapter describes the olivine experiment itself and outlines the sample analysis,drawing a line under these experimental results and adding recommendations for futurework.

Contents

1. Introduction 21.1 The purpose of a Mars Environmental Chamber . . . 2

1.1.1 Other Mars Environmental Chambers . . . . . . . . . . . 31.2 The reddish color of Mars . . . . . . . . . . . . . . . . . . . . . . 4

1.2.1 Where does the reddish color of Mars come from? . . 41.2.2 Olivine occurrence in the Solar System . . . . . . . . . . 61.2.3 Nano-phase Oxides . . . . . . . . . . . . . . . . . . . . . . . . . 8

2. Supporting theory and applications 10

2.1 The Martian atmospheric composition . . . . . . . . . . . 102.1.1 Composition of the Martian atmosphere . . . . . . . . . 102.1.2 The Martian analogue atmosphere (MAA) . . . . . . . . 112.1.3 Monitoring the Martian analogue atmosphere . . . . . . 122.1.4 Residual gas analysis . . . . . . . . . . . . . . . . . . . . . . . 13

2.2 Quadrupole mass spectrometry . . . . . . . . . . . . . . . . . 152.2.1 The quadrupole mass filter (QMF) . . . . . . . . . . . . . 162.2.2 The operation principle of the QMF . . . . . . . . . . . . 162.2.3 Stability conditions . . . . . . . . . . . . . . . . . . . . . . . . 172.2.4 Mass selectivity . . . . . . . . . . . . . . . . . . . . . . . . . . . 192.2.5 Mass spectrum . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192.2.6 Gas ionization . . . . . . . . . . . . . . . . . . . . . . . . . . . . 212.2.7 Lattice ion source . . . . . . . . . . . . . . . . . . . . . . . . . . 222.2.8 Field-axis technology . . . . . . . . . . . . . . . . . . . . . . . 222.2.9 Ion current and fractal distribution . . . . . . . . . . . . . 232.2.10 Ion current detectors . . . . . . . . . . . . . . . . . . . . . . . 24

2.3 Operating the PrismaPlus QMS . . . . . . . . . . . . . . . . . 252.3.1 Operation conditions . . . . . . . . . . . . . . . . . . . . . . . 252.3.2 Data analysis system . . . . . . . . . . . . . . . . . . . . . . . 252.3.3 Technical data of the QMS . . . . . . . . . . . . . . . . . . . 26

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2.3.4 Mass scale calibration of the QMS . . . . . . . . . . . . . . 272.3.5 Coarse tuning of the mass scale . . . . . . . . . . . . . . . . 282.3.6 Ion source calibration . . . . . . . . . . . . . . . . . . . . . . . 29

2.4 Ultraviolet radiation on Mars . . . . . . . . . . . . . . . . . . . 302.4.1 Solar radiation . . . . . . . . . . . . . . . . . . . . . . . . . . . . 302.4.2 The UV flux at the upper atmosphere of Mars . . . . . 312.4.3 UV light in the NEW_JMMC . . . . . . . . . . . . . . . . . 33

2.5 The pressure and temperature at the surface of Mars 332.5.1 Simulated pressure inside the NEW_JMMC . . . . . . 34

2.6 The cooling system of the NEW_JMMC . . . . . . . . . 36

3. Experimental set-up 38

3.1 The architecture of the NEW_JMMC . . . . . . . . . . . 383.1.1 Improvements brought to the old JMMC . . . . . . . . . 383.1.2 The Glove Box . . . . . . . . . . . . . . . . . . . . . . . . . . . . 413.1.3 Inert gas purification and regeneration system . . . . . 423.1.4 Creating an inert atmosphere . . . . . . . . . . . . . . . . . 433.1.5 The oxygen and moisture probes . . . . . . . . . . . . . . . 433.1.6 The antechamber . . . . . . . . . . . . . . . . . . . . . . . . . . 443.1.7 Other specifications of the glove box . . . . . . . . . . . . 453.1.8 The main chamber . . . . . . . . . . . . . . . . . . . . . . . . . 463.1.9 Volume of the main chamber . . . . . . . . . . . . . . . . . . 473.1.10 The vacuum system . . . . . . . . . . . . . . . . . . . . . . . . 493.1.11 The Back Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . 493.1.12 The Turbomolecular Pump . . . . . . . . . . . . . . . . . . . 503.1.13 The support of the chamber . . . . . . . . . . . . . . . . . . 513.1.14 The sample support . . . . . . . . . . . . . . . . . . . . . . . . 52

3.2 Operating procedures . . . . . . . . . . . . . . . . . . . . . . . . . 533.2.1 Operating the valves . . . . . . . . . . . . . . . . . . . . . . . . 533.2.2 Operating conditions . . . . . . . . . . . . . . . . . . . . . . . 553.2.3 Purging the glove box . . . . . . . . . . . . . . . . . . . . . . . 553.2.4 High vacuum creation procedure . . . . . . . . . . . . . . . 563.2.5 Helium leak detection . . . . . . . . . . . . . . . . . . . . . . . 58

3.3 Workplace safety and maintenance . . . . . . . . . . . . . . 593.3.1 Workplace hazards . . . . . . . . . . . . . . . . . . . . . . . . . 593.3.2 Changing the oil of the back pump . . . . . . . . . . . . . 633.3.3 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

4. Preliminary results 66

4.1 The olivine experiment . . . . . . . . . . . . . . . . . . . . . . . . 664.1.1 Handling the olivine samples . . . . . . . . . . . . . . . . . . 66

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4.1.2 Mounting the olivine on the sample holder . . . . . . . . 674.2 Irradiation of the samples . . . . . . . . . . . . . . . . . . . . . . 68

4.2.1 Limitations of the experiment . . . . . . . . . . . . . . . . . 684.3 Sample analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69

5. Conclusion and recommendations 825.1 Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 825.2 Recommendations . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83

6. Appendices 92

6.1 Appendix A . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92

6.2 Appendix B . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96

6.3 Appendix C . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99

1Introduction

1.1 The purpose of a Mars Environmental Chamber

Nowadays, the exploration of the Solar System, and especially of Mars, have developedsignificantly. The apparent similarity between Earth and Mars has been a major driverfor the early space exploration of the Red Planet [12].

To observe and study Mars, the technology has been improved to such a level thattransmissions made at a constant rate by orbiters, landers and rovers are sending databack to the Earth. Due to the availability of more accurate and detailed informationabout the atmospheric and surface conditions on Mars, it is now possible to create proxy-Martian conditions in the laboratory and subject samples to these conditions [14].

An environmental chamber comes as a necessity when this information transmittedfrom Mars receives certain applicability here on Earth. A Mars simulation facility allowsthe study of different processes confirmed or not to occur on the Red Planet. Also newtechnologies that are currently developed to face Martian conditions need such a place inorder to be tested in advance.

In general, a Martian Environmental Chamber will have as a primary task to simulateas many Martian parameters as possible, as accurately as possible. Usually, the aimedparameters to be simulated are:

• Low pressures of 1-7 mbars

• Atmospheric compositions of 95.3% carbon dioxide combined with very smallpercentages of nitrogen ca. 2.7%, argon ca.1.6% and oxygen and carbon monoxide(the later ones are usually negglected due to their small contributions of 0.13% and0.08%, respectively)

• Low temperatures ranging between aprox. -120oC and 10oC

• UV radiation (anywhere between 200-400 nm)

• Simulated wind storms

Research fields spanning from Biology and Chemistry to Geology, Physics andEngineering can take benefit from these environmental chambers mostly to test the

Introduction 3

effects of certain input conditions on biological samples, machines, types of rocks or toobserve chemical reactions or the dynamics of the Martian atmosphere.

1.1.1 Other Mars Environmental Chambers

To mention a few of the largest environmental chambers from around the world andtheir main research objectives, they are: the Small Mars Chamber and the Large MarsChamber at the Open University in England which are running thermal cycling tests tosimulate the Martian surface and to test large instruments respectively [46]; the MichiganMars Environmental Chamber (MMEC) is determining the conditions at which liquidbrines form on Mars [13], the Mars Environmental Chamber for dynamic dust depositionand statics analysis [18], the Mars Simulation Chamber at the Kennedy Space Centerrecreating Martian conditions has implications mostly in aerochemistry and aerobiology[50].

Fig. 1.1: Photo of the Windtunnel AWTS II taken by the author at theMarsLab, in Åarhus, Denmark

The MarsGroup in Åarhus,Denmark, (http://marslab.au.dk)has some ofthe largest simulationfacilities in the worldin terms of studyingevents happening onthe Martian surface.

TheirMarsLab shelterstwo close-circuitand two open-circuitwind tunnels, wherethe team of scientistscan perform reliableexperiments mostlyconcerning dustdynamics and surfacereactions. Moreover, the MarsLab offers the facility for new equipment meant to functionin Martian-like conditions to be tested there.More information about their environment facilities can be found at http://phys.au.dk/en/research/facilities/planetary-environment-facilities/.

Even though a realistic environment is where all the above mentioned conditionswould co-exist simultaneously and at the same rate as on Mars, this is almost impossibleto accomplish. Most of the time, compromises have to be done during simulations.

http://marslab.au.dk

http://marslab.au.dk

http://phys.au.dk/en/research/facilities/planetary-environment-facilities/

http://phys.au.dk/en/research/facilities/planetary-environment-facilities/

Introduction 4

1.2 The reddish color of Mars1.2.1 Where does the reddish color of Mars come from?

The idea of an Environmental Chamber to simulate conditions at the Mars surfacecomes from the need of having a detailed look at several processes and their actions, i.e.,what could be really happening at the surface of Mars, by creating and maintaining asimulated environment similar to the one found on the surface of the Red Planet. TheMartian conditions are completely different from those found on Earth and this may triggersome different physicochemical processes to take place there.

Fig. 1.2: This image was taken by Mastcam: Right(MAST_RIGHT) onboard NASA’s Marsrover Curiosity

By setting up such a chamber weget the possibility to simulate differentprocesses that have been observed – ormay be active - on Mars. The chamberwill be useful for any kind of simulationin which a carefully controlledatmosphere will be necessary (ultrahighvacuum conditions, controlledgas composition, controlled contentof H2O). The first real simulationexperiment that will be conductedusing this new set-up and which willat the same time serve to demonstratethe capabilities of the chamberwill be an Olivine Experiment.

One of the purposes ofthis experiment is to test a hypothesisabout the possible formation of ironoxides or oxihydroxides on the surfaceof pure minerals, in this case olivine,and if successful the results of theexperiment will tell us to what extent weathering of olivine could be responsible for theformation of this iron oxide or oxihydroxides.

In fact, Mars looks red from space because of the iron oxide[s] (rust) formed at thetop layer of its regolith; although this layer is rarely thicker than a few micrometers, it issufficient when lifted in the form of dust particles into the atmosphere by winds, to coversubstantial areas and occasionally to encircle the entire planet, thus strongly enhancingthe bright rusty color seen from distance.

The first fly-by missions to Mars in the 60’ies seemed to show a barren surface scarredwith craters – and on first look a surprising lack of erosion. Analysis of images showedthat densities of craters were lower than on the Moon and as later images showed clouds,rifted valleys and volcanoes, it was clear that Mars was a place significantly different from

Introduction 5

Fig. 1.3: First X-ray view of Martian soil (Image Credit: NASA/JPL-Caltech/Ames) [9]

the Moon.It was until the landing of the Viking landers in 1976 that the general idea of an

earlier very much more active Mars was supported by images of a planet with large waterreservoirs during its early history when the water would have rained out forming rivers inthe mountains and occasionally caused gigantic catastrophic outflows contributing to theformation of the large rift valley, Valles Marineris.

The signs of activity of life previously thought to exist, were not confirmed by thelanders; however, the soil samples from the surface as well as from 10 cm beneath theimmediate surface were found to be chemically reactive [26] and hydrogen peroxide (H2O2)has been suggested as a possible oxidizer of the Martian surface [51].

Although perchlorate salts were considered as potential oxidants for the organics onMars as well, these were first detected and shown to be present at the polar landing site ofthe Phoenix Lander [23], but until then hydrogen peroxide received more attention alongthe years.

In 2000, Yen et al. [26] have shown using electron paramagnetic resonance spectroscopythat superoxide radical ions (O2

−) form directly on Mars-analog mineral surfaces exposedto ultraviolet radiation under a simulated Martian atmosphere, in the presence of almostneglectable amounts of water vapour. The high reactivity of the soils and the increasedquantity of oxygen released at the soil-atmosphere boundary led the team to successfullyverify the formation of oxygen radicals on natural mineral surfaces, choosing labradorite,a plagioclase feldspar, for their experiments.

This confirmed the idea that oxidation can indeed occur without water molecules beingpresent and revealed the possibility of reactive oxygen radicals to form on mineral surfacesunder a high intensity UV flux.

More recently, the experiments performed on soil samples scooped at the Rocknestaeolian deposit by the CheMin instrument on Curiosity in 2012 through X-ray diffraction,confirmed the presence of aproximately 55% crystalline material consistent with a basalticheritage [10] (igneous rocks) including plagioclase, olivine, augite, pigeonite and smallamounts of magnetite and anhydrite and possibly hematite as non-igneous minerals. Alongwith these crystalline phases, the chemical and mineralogical analyses indicate that almosthalf of the <150 µm fraction comprises amorphous material [15] (see Fig. 1.3) [44]).

The importance of the amorphous component with respect to iron-compounds is givenby its composition which apparently contains approximately 23% FeO + Fe2O3, suggesting

Introduction 6

that ferric nanophase oxide (npOx) is present in abundance [10]. Additionally, it is thoughtthat the amorphous component contains also molecules such as H2O, SO2, CO2 and O2and further evidence revealed that water molecules primarily can be found within theamorphous component [15].

Also, further evidence that came with the most recent data received from Curiosity,indicated a significant water abundance in common average soil (1.5 to 3 weight percentin samples from the Rocknest wind deposit) [17]; in addition, the released temperaturesuggested that H2O is bound within an amorphous component of the sample [44].

What it is known with certainity is that the granular size of the particles means a largearea vulnerable to chemical reactions along the entire planet’s surface and it is probablya feature of their composition that allows oxidation to happen, most likely when a highintensity UV flux is also present. An important feature of the smallest particles – withthe largest specific surface area – is that these are most prone to become airborne – andbeing airborne the cross-section for interaction with UV-radiation is strongly enhanced.But, how are these smallest particles formed in the first place? Are they relics from anearlier epoch on Mars? – or are they continuously formed by a process which is still activeeven today?

Throughout our experiment, the aim is to study and try to identify any possiblereactions that could occur on the surface of pure minerals, for example olivine samplesirradiated by the intense UV flux. Experiments like this can now be performed inside theNEW_JMMC, and we may be able to conclude whether or not the UV light is able tobreak down the minute amount of water from the nano layer at the surface of theMartian minerals, possibly converting this layer into an effective oxidizing factorattacking the intrinsic iron atoms of the pure minerals.

1.2.2 Olivine occurrence in the Solar System

Olivine is a silicate mineral usually found in many mafic igneous rocks. In fact, olivineis the common name for a suite of iron-magnesium silicate minerals known to crystallizefirst from magma [36].

The end-members of this suite are characterized by the highest concentration ofmagnesium within the mineral, named forsterite, and the highest concentration of iron,named fayalite, respectively. However, the two end members in pure form are relativelyrare and most of the minerals in this suite contain both iron and magnesium in differentamounts. Compositions of olivine are commonly expressed as molar percentages offorsterite (Fo) and fayalite (Fa) [37]. Along with magnesium and iron, olivine alsocontains oxygen and silicon. Additionally, manganese and nickel are often found inrelatively small quantities; however, the later is strongly responsible for the color of themineral. It can change though into a reddish color once olivine interacts with water, andconsequently weathers into clays or iron oxides. Depending on the ratios of thecomponent atoms, i’s color can have all shades of yellowish green or greenish black.

Olivine is a rock-forming mineral which occurs in mafic rocks and ultramafic (silica-poor) igneous rocks such as basalt, gabbro, troctolite and peridotite. Dunite, for example,is a rock composed exclusively of olivine [37]. There are a few other names given to olivine,for example chrysolite, meaning ”Golden Stone” in Greek or the French name, peridot.

Introduction 7

Fig. 1.4: Different types of olivines and their sources as exposed at the Geological Museum(Copenhagen) 1.Olivine (Mg, Fe)2[SiO4], Eifel; 2, 3.Almklovdalen peridotite, Norway;4.Olivine, St. John Island, Egypt; 5.Peridotite, Icohistan, Pakistan; 6.Olivine, Vesuvio;7.Hyalosiderit, Kaiserstuhl, Bresgau; 8.Fayalite Fe2[SiO4]

Nowadays, there is a particular focus on olivine because it reacts exothermally withCO2 and forms secondary minerals, including carbonates. Therefore it is considered apromising phase for carbon sequestration, to convert carbon dioxide from the atmosphereto mineral form [21]. Since the main elements which make up the crystalline structure ofolivine are magnesium, iron, silicon and oxygen it is understandable why this mineral isone of the most abundant on the surface of Earth. It usually forms in mafic igneous rockswhere it partially makes up the rock′s structure, i.e. basalt, gabbro, or ultramafic rocks,where in some cases it can almost entirely form the rock, i.e. peridotite.

More than 50 per cent of the Earth’s upper mantle consists of olivine and it is generallythought that mantle-derived melts are generated in equilibrium with this mineral [24].However, its occurrence is not limited to the Earth; it is present in many different type ofsolar system material, from microscopic interplanetary dust particles to asteroids [3] andterrestrial planets.

Olivine was identified by Earth-based telescopic observations at two craters on thenear side of the Moon, on the concentric regions around the South Pole and on the impactbasins where the crust is relatively thin [25]. Its presence has also been identified on certaincomets and asteroids, mostly from the inner part of the Solar System.

Olivine has also been detected in meteorites; pallasites are a class of meteorites, beingcomposed of relatively equal amounts of olivine and nickel-iron structures, respectively.Pallasites originate near the metal-silicate boundary of differentiated asteroids andrepresent the interface, where the metal and silicates are physically intermixed. Theresult is beautiful structures in which the (almost) transparent olivine may be present asmacroscopic inclusions in (stainless) metal.

More detailed information about the properties of the olivine can be found in Table 1.In Fig. 1.4 are shown different minerals belonging to the Olivine Group. The photos

were taken by the author at the Geologic Museum, Copenhagen.

Introduction 8

1.2.3 Nano-phase Oxides

Nano-phase oxides could have formed through several processes on the surface of Marsand it is very likely that a combination of two or more of these processes happened intime.

As a first hypothesis, nanophase oxides could have formed by dissemination ofdegradation products of palagonite. Palagonite may form by quenching (ultra-rapidcooling) of igneous material when this erupts into a large, cold, body of significant heatcapacity, which could be either a glacier or a lake. Processes like this have taken place onHawaii and Morris et al. [19] have indeed suggested that processes similar to these couldbe the origin of the nanophase oxides on Mars [19].

Secondly, photolysis (or photodissociation) might have created np-oxides; because ofthe low density of its atmosphere and the lack of an ozone layer, Mars is highly exposedto intense ultraviolet fluxes that reach all the way down to its surface and can break downthe molecules of water vapor or surface films resulting in new radical elements ready toreact with the iron within the surface minerals.

Thirdly, it is likely that chemical weathering happened through the direct reactionbetween minerals and water, resulting carbonates, clays or iron oxides. Usually, thewater implied in the reaction is acidic and gives away free hydronium-ions (H3^+) andhydroxide (OH)− ions which may chemically attack minerals, thus forming secondarymineral structures. The most important types of chemical weathering are hydrolysis,oxidation and carbonation. Each one of these processes transforms the original mineralinto a new mineral depending on which elements is water reacting with.

Olivine can undergo both oxidation and hydrolysis weathering, depending on theconcentration of magnesium or iron within the mineral. The upper parts of the Martianmantle are composed chiefly of olivine and its higher pressure polymorphs, wadsleyiteand ringwoodite. These phases are known to be capable of chemically incorporatinglarge amounts of H2O as hydroxyl [33]. However, the storage capacity of olivine in theMartian mantle may be quite different, as it is richer in FeO [52].

One goal of the olivine experiment in the NEW_JMMC apart from validating thechamber, is to observe the bahvior of freshly cleaved olivine surfaces and hopefully be ableto detect the effects from the UV flux on the pure mineral’s surface.

2Supporting theory and applications

2.1 The Martian atmospheric composition2.1.1 Composition of the Martian atmosphere

The atmosphere of Mars has changed composition dramatically throughout the planet’shistory. In terms of density, the Martian atmosphere has become much thinner, affectingthe pressure and the temperature at different atmospheric levels; therefore, water in liquidstate became unstable under such conditions. Whilst many theories try to explain whatcaused the loss of almost the entire atmosphere of Mars throughout and back in the history,both remote and in-situ measurements have detected with relatively high precision thepresent amount of component gases. (Fig. 2.1).

Mars Express (ESA, 2003) was equipped with instruments with the ability to study thecomposition of the Martian atmosphere and in particular which species are continuouslybeing lost from the atmosphere. Recently two missions have been sent to Mars withthe aim to study atmospheric loss: The Indian Space Research Organisation launchedMangalyaan and NASA launched the MAVEN mission, both in 2013.

Carbon dioxide gives the largest percentage, around 95.9%, of the atmospheric mixture.However, the amount of carbon dioxide detected in the atmosphere varies considerablythroughout the Martian year, most notably when strong winters occur on one of the poles,where a significant part of the atmosphere may condensate into dry ice, reducing somehowthe atmospheric CO2 quantity, while during the summer, it sublimates back into theatmosphere. The condensation-sublimation cycle changes the surface pressure with up to25%.

The mixing ratios of CO2, N2, Ar, O2, CO, Ne, Kr and Xe on the Martian surface werealready determined in 1976 when the Viking Landers reached the surface of Mars, analyzingits atmosphere. A small amount of water vapor in the atmosphere of Mars, which variesseasonally, has also been detected and this small water content has several times beendetected as surface frost by landed missions [20]. Consequently, from early observations anumber of minor constituents that arise from the interaction of solar radiation with watervapor and carbon dioxide have been revealed, namely: carbon monoxide, atomic oxygen,molecular oxygen, ozone and atomic hydrogen [4]. The most recent in situ measurements

Supporting theory and applications 11

Fig. 2.1: Mass spectrum of the Martian atmosphere with mass peaks labeled for the mainatmospheric species [16]

done by the Curiosity rover, a tunable laser spectrometer (TLS) and a quadrupole massspectrometer (QMS) are currently used to obtain a more detailed overview of the Martianatmosphere. Spectrometric analysis of these compounds carried on by Curiosity duringits first experiments on Mars, revealed more precise volume mixing ratios for the mostabundant gases: Carbon dioxide, 0.960(±0.007); 40Ar, 0.0193(±0.0001); nitrogen, 0.0189(±0.0003); oxygen, 1.45(±0.09) x 10−3; carbon monoxide, < 1.0 x 10−3 and 40Ar/36Ar,1.9(±0.3)x103 [16].

2.1.2 The Martian analogue atmosphere (MAA)

One of the improvements meant to be done on the NEW_JMMC set-up was to createa realistic Martian analogue atmosphere (MAA) and sustain it for as long as possible.

The main component of the atmosphere on Mars is carbon dioxide [roughly 96%].Initially, the idea of introducing the required quantity of gas into the chamber was to dropin a few pellets of dry ice (supplied by the HCØ Institute) and simply let them sublimate ina container directly connected to the main chamber. The major advantage of this methodwould have been the complete freeze out of the existent water vapors caused by the verylow temperature of the ice (aprox. -78.5oC). Nevertheless, the method would have beenrather tedious and probably not very efficient in terms of handling the pellets. Therefore,another method of inserting the gas into the reaction chamber was used.

A 20l CO2 cylinder has been directly connected through a silicon rubber hose to thebottom inlet line of the chamber and controlled through a tap valve until the pressureinside increased up to Martian levels. Although the chamber was filled in with pure CO2through the main line connected to the CO2 cylinder, small amounts of residual gaseswere also present. These gases were subsequently released through the outgassing of thechamber’s walls and not removed by the vacuum pumps. Their low concentrations, stillmade up a pressure of -0.865 mbar prior to the injection of the CO2.


2.1.3 Monitoring the Martian analogue atmosphere

Recreating the exact Martian atmospheric composition inside the environmentalchamber is definitely still an idealistic concept. The major insufficiency that will notallow the desired gas content to exist inside the NEW_JMMC, is not the incapacity ofpumping inside pure CO2 but the difficulty of removing existent residual gases stuck inthe chamber’s walls and which will keep outgassing long after a standard vacuuming ofthe chamber is done. On the other hand, leaks will occur around the set-up at vulnerablespots such as damaged fittings or imperfectly sealed feed through, resulting in theinfiltration of undesired gases which alter the quality of the vacuum.

Therefore, water molecules will be present in considerable larger amounts than theycan be found in the Martian atmosphere; molecular nitrogen will also show up in highpercentage as it is the most abundant gas in the terrestrial atmosphere. One way oftrying to diminish these gases (i.e water vapor and molecular nitrogen) is by takingadvantage of the high intensity Xe lamp that can emit strong UV radiation inside thechamber. What happens when the fraction of UV light with wavelength around 200nmhits the gaseous molecules is called photodissociation and how these molecules breakthrough photodissociation is depicted in eq. (2.1) and (2.2).

N2 + hν → N +N (2.1)

H2O + hν → H +OH (2.2)

With a continuous pumping of the chamber during the first stages of the measurements,it is expected that partially, atomic hydrogen and nitrogen respectively, resulting from thephotodissociation process, will be ejected from the system. However, regardless of what ishappening with the free ions, the hydroxyl radical, OH, will be available for new reactions.

Finally, following the 2-3 hours of such stress being applied to the gases inside theNEW_JMMC, pure CO2 is injected directly from the CO2 line, up to a pressure of 10-20mbar which exceeds with only a slight difference the average pressure range present onMars. The operating procedure of the valves during the injection of CO2 is completelydescribed under the 3.2.4 High vacuum creation procedure section.

Fig.2.2 shows the CO2 peak (amu=44) that increases significantly when a small amountof gas from the reaction chamber was transferred to the analyzing chamber. Only the righthalf of the spectrum is realistic and that is because the amount of CO2 stays such a shortfraction of time in the analyzing chamber before it is ejected by the vacuum system, thatthe QMS doesn’t have enough time to complete a full scanning.

In the same manner, Fig.6.5 and Fig.6.6 clearly shows how the Argon peak increasedafter the glove box has been flushed two times with this gas. The sensitive QMF detectedthe argon infiltrated through the chamber’s leaking spots after the vacuum was created.This was not a good news though because it confirmed once again the fact that the systemhad small leakings.


Fig. 2.2: Gas composition spectrum after the injection of CO2 into the chamber

2.1.4 Residual gas analysis

Although vacuum pumping systems have an increased performance when it comes tocreate highly purified environments, it is difficult to completely eliminate contaminationat very low levels.

The main task of quadrupole gas analyzers is to measure this contamination.A well-calibrated detector can provide valuable information about the detected amount

of residual gas, avoiding in this way the guesswork that previously has been widely usedin vacuum technologies.

We found ourselves in the need of measuring the exact quantity of residual gasesexistent in the NEW_JMMC volume; monitoring this quantity becomes very importantwhen the quality of the vacuum has to be stated.

The PrismaPlus QMS implies an open ion source which will be at the same pressureas the rest of the vacuum system once attached to the analyzer chamber. The maximumoperating pressure is 10−4 torr (10−5 mbar). The minimum detectable partial pressure(typically measured for N2 at 28 amu) is as low as 10−14 torr for units equipped with anelectron multiplier. Higher pressure results in a decrease in sensitivity due to space chargerepulsion between ions [49].

An open ion source (OIS) means that the filament and the anode are in direct contactwith the surrounding vacuum, so that the pressures in the ionizer, the analyzer and thedetector are equal with the chamber pressure.

In the absence of an inert atmosphere created in the glovebox, the PrismaPlus QMScould have also been used as a helium detector. By pumping helium around the set-up, itcould have been detected inside the chamber by spectrometric measurements, as leaking


would have happened through vulnerable spots. However, this procedure has been skippedbecause the minute amount of argon that may enter into the chamber is not sufficient tocompromise the on-going experiments.

The most straightforward method used to remove residual gases that usually cannotbe removed even by creating a high vacuum, is baking out the entire volume. By heatingthe chamber up to 200oC, any remnant water molecule can be detached from the wallsthrough vaporization and eventually ejected through the vacuum system. Usually, watermolecules are the most abundant and a bake out at 200oC would be more than sufficientto vaporize them out. The NEW_JMMC is bake-able up to the point when the pressuretransducer, cooling system and wires are inserted. The metallic structure of the entireset-up, the QMA and the VITON O-rings used for each flange connections can allow suchhigh temperature to exist without any damages. However, baking isn not yet possible forthe present configuration, where the electronics mutually permit a maximum temperatureof 85oC.

Baking out the chamber means that no other further contamination is permitted.Inserting back-up samples or adjusting the sample tray would take a few minutes withthe inert atmosphere creating a protective shield between the chamber’s volume and thesurroundings, while installing the electronics would imply at least a couple of hours of openchamber and open glove box which will definitely compromise the baking-out process andrecontaminate the interior of the reaction chamber.

However, a temperature close to 85oC existed in the chamber when the Xe arc lampwas used to irradiate the samples. Using the ideal gas law and knowing the initial pressure,the final pressure (both indicated by the pressure transducer), the initial temperature wasconsidered to coincide with the room temperature, so that calculating the final temperaturewhich increased due to the heating produced by the lamp, was trivial.

During the experiment, the lamp was turned ON in cycles of a couple of hours untilthe temperature approached the maximum value of 85oC, supported by the transducer,when the lamp was turned OFF for 1-2h to permit the cooling of the system.


2.2 Quadrupole mass spectrometry

Mass spectrometry is an analytical method extensively used to determine the molecularmass of different gases, to individually describe the chemical structure of each elementwithin a mixture or to perform isotopic analysis of complex samples. It is widely recognizedas a very powerful and valuable gas analysis technology with applications in both researchand industrial fields [27].

By using mass spectrometry real-time gas analysis, one can gain an immediate insightover the chemical composition of a sample through partial pressure measurements. Thismethod is more efficient than the one where total pressure measurements were implied.

Small, easy to handle mass spectrometers, like the one attached to the NEW_JMMC(Fig. 2.3), used in vacuum equipment are also called residual gas analyzers (RGAs).They can be used up to UHV conditions, where they achieve ppm levels, or to detectleaks.

Fig. 2.3: Photo of the PrismaPlus QMS attached to the NEW_JMMC taken by the author

A Quadrupole Mass Spectrometer (QMS) is made up by an ion source, connected to thegas container through an inlet system, a mass filter (analyzer) and a detector; the outputis given by the data analysis system via a specialized software. All these component-partsare presented in the following sections, where a more detailed overview of the operatingprinciples and the output of the quadrupole mass spectrometer (QMS), the conditionsthat have to be met in order to run it safely and the spectra of the investigated gases aregiven.


2.2.1 The quadrupole mass filter (QMF)

The analyzer of a Quadrupole Mass Spectrometer (QMS) is usually mentioned as aQuadrupole Mass Filter (QMF) due to the fact that it acts rather as a mass filter thanas an energy or momentum spectrometer [7]. It is actually a mass filter for positive andnegative ions with particular mass-to-charge ratio.

Because predicting the ions trajectories in a QMF is not a trivial work at all,quadrupole mass spectrometers are considered very complex devices.

2.2.2 The operation principle of the QMF

A Quadrupole Mass Filter is made up of four quadrupole rods (electrodes), parallel toeach other and positioned in a square configuration (Fig 2.4). Although the ideal shape oftheir cross section would be a hyperbolic one, due to manufacturing reasons it is usuallycircular with subsequent corrections done in order to obtain an ideal electric field.

It has been shown that the best approximation to the ideal hyperbolic field can beobtained if the radius of the circular rodes (r) is related to the quadrupole field radius (r0)by the expression:

r = 1.148r0 (2.3)

[7]Each two opposite rods are interconnected and for each of them a DC voltage UDC

and a high-frequency, voltage RF are applied, so that two rods have a positive voltage

+ U = +UDC +RFcos(ωt) (2.4)

and the other two have a negative voltage

− U = −UDC −RFcos(ωt) (2.5)

The DC and the high-frequency voltages are applied separately for each pair ofinterconnected rods, creating an electrical quadrupole field between them.

While ions with different mass enter the electrode system, the amplitude and frequencyof the RF voltage and the ratio between the amplitudes of the RF voltage and the DCvoltage (RF/DC) will determine that only certain ions, having a specific mass to chargeratio m/e, will move all the way between the rods and eventually reach the detector. Theseions will be referred as the ones moving on stable trajectories. Every other ion travellingthrough the rods and which will collide with them is attributed with an unstable trajectory;these ions will never make it through the detector.


Spanning over more m/e values means a constant variation of the voltages; this is theway how mass spectra are obtained.

Under the quadrupole field’s influence, both stable trajectory ions and unstabletrajectory ions describe a helical motion along the direction of the Z axis, parallel to therods.

Fig. 2.4: The Operation Principle of a QMF (Image Credit:Pfeiffer Vacuum on-line Compedium)[28]

2.2.3 Stability conditions

The motion of the ions is generated by the electric field between the rods of the analyzer.The field acts as a restoring force which constantly pulls the deviated ions towards thecenter of the analyzer. This motion is mathematically described by how is the potentialdistributed within the analyzer and how does it affect the entering ions.

The solutions of the Mathieu’s differential equations show very precisely how are theions moving within the quadrupole field. In this section, resolving these equations wasskipped as it can seem a bit sinuous and it does not make the point of this paper.

The basic idea behind these differential equations is that the solutions are being eitherbounded or unbounded. A bounded solution refers to the situation when an ion travellingthrough the quadrupole field would make its way all along the detector, thus describinga stable trajectory, whereas an unbounded solution refers to a strongly displaced particlewhich would never make it through the detector, having an unstable trajectory.

An extended analysis of the differential equations reveals that the stability of theappropriate solutions depends only upon two parameters a and q which are defined below.


a = 8eUDCmr2

0ω2 (2.6)

q = 4eVmr2

0ω2 (2.7)

Fig. 2.5: Stability diagram of a QMF (Image Credit: Pfeiffer Vacuum on-line Compedium)[28]

As shown in Fig.2.5, the stability region located beneath the two red curves representsthe stable area with oscillation amplitudes of less than r0 and is called the a-q space [28] .The blue line is called the work characteristic of the mass filter (or the slope of the massscan line) and is obtained by dividing the equations (2.6) and (2.7) by one another.

a

q= 2(UDC

V) (2.8)

Only the small triangle area between the two curves and the work characteristic isassociated with the ions which will eventually make their way through the detector. FromEq. 2.8 results that the condition U

V = a2q < 0, 1678 has to be valid to actually have a

detection of ions.Note: Some of the spectra images presented in this chapter are also attached in full

page size in Appendix C due to the fact that the captions cannot be easily readable in theimages inserted in the text files.


2.2.4 Mass selectivity

As it can be deduced from Fig. 2.5, when no DC voltage is applied to the rods, theywill run exclusively on the time-dependent RF voltage applied to them, so that the acoordinates will be zero and a signal will show up only along the q axis. In this situation,all ions having the mass-charge ratio larger than a threshold value will be passing throughthe device; by increasing the amplitude but maintaining the frequency of the RF voltageconstant, larger values of the mass/charge ratios will be allowed through the device.

This outlines partially how the mass selection works at a QMF. For a full efficiency ofthe device, DC and RF voltages will be applied together and increased at the same rate.Because one pair of rods is connected to a positive voltage and the other to a negativevoltage, each pair of rods will put out a total voltage (DC+RF) signal opposite in phaserelative to the voltage signal of the other pair of rods.

The benefit of using two voltages is that an extended scanning over various mass/chargeratio ions can be done. The more powerful RF voltage will affect mostly the lighter ions,driving them either towards the rods or outside the quadrupole system so that they arefiltered out, while the DC voltage has a strong influence over the heavier ions in the sensethat most of them will be put on unstable trajectories [6].

Applied simultaneously, these voltages act like two filters, a low-mass filter and a high-mass filter respectively, and the ratio between them can be set in such a way that therange of mass/charge ratios can be minimized to a single value.

When this ratio is constantly increased by equal values, a complete scan in terms ofmass/ratio values can be performed in order to obtain a mass spectrum.

2.2.5 Mass spectrum

A mass spectrum is defined by the American Society for Mass Spectrometry as aspectrum obtained when a beam of ions is separated according to the mass/charge ratiosof the ionic species contained within it [39].

In order to obtain a spectrum of a gas sample, periodic scans are done at certain speedrates and the obtained data is being recorded usually by the computer connected to theanalyzer.

Each mass number in the spectrum is scanned within a very short allocated periodof time and is being plotted against the ion current corresponding to every single gascomponent; this is efficient when all masses have to be known to the same extent as ithappens at the scans taken by the PrismaPlus QMS.

Fig. 2.6 and 2.7 represent the air spectrum both as a Faraday analog spectrum andas a Faraday stair (bar) spectrum. The stair spectrum advantage over the Faraday one isthat it displays the values discreetly, using less data storage memory.


Fig. 2.6: Faraday stair spectrum of air taken with the PrismaPlus Mass Spectrometer inside theNEW_JMMC at a pressure of -0.865 mbar

Fig. 2.7: Faraday analog spectrum taken with the PrismaPlus Mass Spectrometer inside theNEW_JMMC at a pressure of -0.865 mbar


In the right bottom corner of the two plots, the Spectra Library is being shown as avery convenient facility of the Quadera software; the spectra shown in Fig. 2.6 and 2.7were taken for a sample of air. The air main masses are highlighted with blue so that theconnection with the spectra peaks can be easily observed.

Further scanning will be done once a high vacuum is created inside the chamber andCO2 is let into the system. By observing the spectral scans in real time it will bepossible to correct the volume of CO2 whenever it will be needed.

2.2.6 Gas ionization

Prior to entering the mass filter, the analyzed gases are passed through an ion sourcewhere they are bombarded by a flux of electrons, thus becoming ionized. The ion sourcesits on the top of the mass filter and usually consists of a pair of filaments, a source heaterand a temperature sensor (Fig. 2.8).

Fig. 2.8: Photo of the PrismaPlus QMS’s analyzertaken by the author

The filaments (cathodes) of thesource will be heated up and eventuallyemit electrons which will be acceleratedby a voltage applied between the anodeand the cathode. Neutral gas moleculesenter the formation area in this regionand are ionized by collisions betweenelectrons, forming single- and multiple-charged positive ions [28].

The number and the type of theresulting ions is strongly related tothe voltages applied in order to createthem. The higher the accelerationvoltage applied is, the larger the numberof emerging ions will become.

Besides the expected ions formedthrough electron bombardment of theinitial molecules, other types of ions,which can be fractal or recombinationions, are also formed.

The PrismaPlus QMS is equippedwith this robust and highly sensitive ionsource, which is especially suitable forresidual gas analysis.

The ion sources of the QMSs canbe of several types: axial, lattice,crossbeam or gas-tight ion sources.Our device has attached an ion sourcesimilar to the lattice type and has twocathodes.


2.2.7 Lattice ion source

The PrismaPlus 220 QMS attached to the NEW_JMMC has a lattice ion source. Thedesign of this kind of source is a relatively simple one; the top of it is a grid cage with thedirection of the grids parallel to the principal axis of the quadrupole and with two tungstenfilaments (cathodes) installed outside, but in the very close proximity of the cage.

Having two cathodes means that this ion source can afford particularly secureoperation [29] and the whole easy-to-dismantle structure permits quicker cleaning andfilament replacing operations.

This type of source is the most frequently used when it comes to gas analysis in highor ultra-high vacuum. The vacuum around the analyzer in the NEW_JMMC whilerunning will be approximately -0.865 mbar.

2.2.8 Field-axis technology

Fig. 2.9: Field-axis technology (Image Credit: The New MassSpectrometer with the Added Plus! Modular Design.Powerful Software. Wide Range of Applications.)

Field axis-technologyhas been implementedinto the PfeifferQMS because it providesa safer transmissionof the ions between the ionsource and the mass filter.This technology minimizesthe interaction of the ionswith the peripheral fields,enhancing the sensitivityof the device without theneed of filters, increasingits performance. InFig. 2.9 the well collimatedion beam is presented along

with the energies of the flux between the ion source and the mass filter.


2.2.9 Ion current and fractal distribution

While the gas molecules and atoms exist between the anode and the cathode of theQMS (the formation space), they get ionized by being bombarded with low-energyelectrons, resulting single and multiple positive ions. The collection of ionized gasmolecules emerging from an ion source is referred to as an ion current.

The ion current is measured in [A] and for a gas component K it can be calculatedfrom the following equation:

IK+ = i_ · Ie · s · pK (2.9)

Where: i_ = electron current (emission current), in Ale = mean path length of the electrons, in cms = differential ionization effect cross section K, in 1/(cm ·mbar)pK = partial pressure of the gas component K, in mbar [29]

The differential ionization indicates the number of ions produced by one electron on apath of 1 cm at a given gas temperature and a pressure of 1 mbar.

A current of 1nA (10−9) corresponds to the arrival of several billion singly chargedions per second at the detector (Faraday cup). By doing the calculation, knowing that1A corresponds to a current of 1 C/s:

10−9x([1C/s]x(1ion)/1.6x10−19C) = 6.25x109ions/s (2.10)

When spectra is taken with the PrismaPlus QMS, the intercepted ion current fromthe different residual gases is between 0.50 and 9.5 nA (or [E-09 A]). To draw a picture ofhow small this current is, it can be compared with a current flowing through a 60W bulbconnected to 120V which measures 0.5 A.

The electron bombardment gas ionization described above is a complex process as thenumber and type of the resulting ions depends strictly on the energy carried by theimpact electrons. It has to be taken into account that apart from the ions with single ormultiple charges, fractal ions also occur. The scheme describing the types of thesefractals for an example molecule ABC, is:

ABC + e− → ABC+ + 2e−ABC++ + 3e−AB+ + C + 2e−BC+ + A + 2e−

A+ + BC+ 2e−

C+ + AB+ 2e−

B+ +A + C + 2e−


2.2.10 Ion current detectors

In quadrupole mass spectrometry it is preferable to have an ion current flowing intothe analyzing system because it can get easily manipulated by the quadrupole field createdbetween the rods. In this section, the focus is put on two types of detectors, the ones usedby the PrismaPlus QMS, and their behaviour after being reached by the ion currents. Eachof them has advantages and disadvantages depending on the purpose of the measurementthey are used for.

• Faraday CupA Faraday cup is the simplest type of detector able to detect ion currents withintensities between 10−14 and 10−9 A, to convert the current to voltage by usingan electrometer amplifier and to send the output signal towards the data analysissystem. Basically, a metallic cup gets electrically charged when it is bombardedby the ions emerging from the quadrupole field. Hence, a small current which willeventually give an output depending on the collected charges, is formed.The most important advantages of the Faraday cup are: its simple structure, itsstability for long periods of time and capacity to run at high temperatures; however,the major weaknesses of this type of detector are the inability to detect small ioncurrents or to provide very fast measurements.

• Secondary Electron Multiplier (SEM)For small ion currents the secondary electron multiplier is generally used.The basic physical process that allows an electron multiplier to operate is calledsecondary electron emission [38]. The more complex structure of this detector ismade out of a set of cylindrical metal sheets (12 up to 24) being consequently disposedso that the incident beam of electrons hits the surface of these metal sheets, causinga sudden emission of secondary electrons which will follow a zig-zag trajectory. Thespeed of the electrons is increased by applying high voltages so that an amplificationof 107 can be achieved; this implies low partial pressure interception.The weakness of this detector is that the coated metal sheets can degrade in timeand thus affect the amplification rates.

Fig. 2.10: Ion detectors: (a) Faraday detector; (b) SEM with discrete dynodes (Image Credits:”Quadrupole mass spectrometry of reactive plasmas”, Journal of Physics D: AppliedPhysics [45])


2.3 Operating the PrismaPlus QMS2.3.1 Operation conditions

It is very important to meet the indicated operation conditions while running the QMS.The chamber containing the analyzer must hold a high vacuum, with pressures of less than10−4 mbar.

The vacuuming system at the NEW_JMMC drops the pressure inside the analyzerchamber down to the order of -0.865 mbar when both the backing pump and the TMP arerunning in tandem. The partial pressures inside the chamber are given by the continuousresidual gas desorption from the walls of the chamber.

The filament of the analyzer is being automatically turned OFF by the safety system ofthe device equipped with a pressure sensor, once the surrounding pressure increases abovethe recommended level. This happened a few times at the NEW_JMMC during the firststages of measurements, after the pumps were stopped and leaks were still occuring aroundthe chamber.

Sudden pressure increases should be avoided while the filament is turned ON, especiallywhen the carbone dioxide (the main component of the MAA) is introduced into the system.

The pressure will be permanently monitorized using the PX409USB pressuretransducer, which measures gauge pressures, installed inside the reaction chamber inorder to have a continuous evidence of the vacuum status, but also to be able to detectany minor pressure variations that could happen while the experiment is running.

2.3.2 Data analysis system

Each operation done by the PrismaPlus QMS is analyzed, stored and displayed to theuser through the Quadera software.

The mass spectrometer is not having any data storage capacity or display, so thatits analyzing system is totally dependent on a connection with a computer and the datatransfer between them is made via Ethernet.

The Quadera software is able to perform a test simulation even without the massspectrometer being installed, therefore the user can become familiar with the interfaceand basic commands prior to the installation of the device. Once the device is set up,the analyzed data during or after the measurement is transmitted to the computer whichdisplays the results through the user friendly interface of Quadera.

The following data are typically displayed:


• Mass spectra with adjustable mass range, linearly or logarithmically calibrated forconcentration;

• Display of the chronological sequence of partial pressures;

• Bar graph measurements to reduce the volume of data [28]

When quantitative analysis is needed, the mass spectrometer has to be calibrated.Quadera also comes with a pre-installed library which provides the fractal distribution

for the most common gases that can be encounterred while analyzing gaseous mixtures.It is actually very practical to go through the library once a spectrum is obtained, andtry to figure out the measured compounds by matching the spectrum peaks with libraryvalues.

A tricky task to solve when the quality of a gas mixture has to be evaluated is toidentify the different airborne particles which result after the gas ionization; for example,carbon dioxide can come out in a spectrum as 12C+ with the mass number=12, 13C+ -mass number=13, 16O+ - mass number=16, 12C16O2

++ - mass number=22, 12C16O+ -mass number=28 and so on and might overlap with other gases that have the same massnumbers. As a major help, the Quadera software has been calibrated with mixtureshaving non-overlapping components so that the concentration or partial pressure of anygas component can be automatically calculated by the software.

2.3.3 Technical data of the QMS

The system of the QMS consists of the electronic unit QME 220, the QMA 200 analyzer,the input/output module IO 220, the SP 220 power supply and a PC running the Quaderasoftware.

Generally, the analyzer comes separately packed and requires special care when handledand attached to the electronic unit. It is sheltered by a sealed plastic cylinder and isrecommended that once the cylinder is removed, the analyzer to be mounted as soon aspossible in a relatively sealed volume (i.e. the analyzer chamber) in order to avoid externalcontamination.

The maximum operating temperature of the QMA 220 is +150oC and its maximumbakeout temperature, with the QME removed, is +200oC.

The mass range u of the QMS attached to the NEW_JMMC is between 1 and 100,having a Faraday detector type, with a minimum detectable partial pressure of <1x10−12

mbar and a maximum operating pressure of 1x10−4 mbar [48]. Sometimes, throughoutthe spectrometric measurements done at the NEW_JMMC, the mass range can appear toextent only to 50; that was preferred because mostly the masses in the range of 1-50 havebeen of interest. However, the range can be extended anytime from the Edit tab underthe spectrum area to any value from 50 up to 100.

The measurements modes are scan analog, scan bargraph and MID where themeasurements speed for the scan analog + bargraph peak is between 20 ms/u and 60ms/ while the speed for the bargraph stair is between 2 ms/u and 60 ms/u. The reasonwhy a bargraph stair measurement can be done faster is because it represents discrete


values and ignore intermediate values which otherwise appear at the continuous analogscans.

The power supply works on 24 VDC / 2.0 A, 47-63 Hz and the control between theQME and the computer is done through Ethernet connection. The analog inputs of theIO 220 module have a 15 pin D-sub connector, working on 5 channels, with a differentialinput configuration. A differential input means basically a way to reduce the noise thatshows up when information is transmitted. It measures the magnitude of an input signalas the difference between two inputs, where one of them carries the basic voltage plus thesignal of interest and the other carries just the basic voltage so that the differencebetween the two yields only the signal of interest [30].

2.3.4 Mass scale calibration of the QMS

Sometimes, at a mass spectrometer, small deviations can occur between the nominalmass number and the real position of the peak maximum. The correction of thesedifferences is done through specific measurements which determine the peak maximumand rearranges its position in order to increase accuracy in further measurements. Whena mass scale adjustment is conducted, it is done via a template which automates thedetermination of measured mass numbers. It can be configured through the RecipeEditor [1].

Fig. 2.11: Ok state of the Mass scale calibration

The alteration of the current status of the mass scale can be done through:

1. Update Mass List – adds new masses to the mass adjust list from the recipe;

2. Remove Mass – removes a selected mass from the mass adjust list;

3. Reset Mass Scale Table – resets all actual masses in the Mass Adjust list to theirrespective Reference Mass.


During the Mass Scale Calibration at the PrismaPlus QMS, the tuning procedureconsisted in resetting the Actual Mass until it matched the Reference Mass and the Okstate was indicated, showing that the calibration has been done. The Ok state can be seenabove, in Fig. 2.11.

Initially, the Peak width too narrow state appeared, which meant that the peaks weretoo narrow in order to determine a maximum.

2.3.5 Coarse tuning of the mass scale

The procedure of mass scale calibration can be done in two steps, coarse tuning andfine tuning, but usually a coarse tuning only is sufficient. During the coarse tuning twoparameters are used to shift and to shrink or stretch the mass scale. Eventually, thiscoarse tuning will be applied to all measurements [1].

Fig. 2.12: Coarse tuning of the mass scale done by adjusting the actual peak positions to thenominal mass numbers

At the PrismaPlus QMS the coarse tuning was conducted as it follows:

• Air was used as calibrating gas so a standard vacuuming of the NEW_JMMC wasdone until the pressure reached -0.864 mbar;

• From the View menu, Show Start Page was selected;

• From the ‘’Calibration and Tuning” list, Mass Scale Tuning (Coarse).qmt wasselected, creating a new calibration project;

• Once the calibration project popped-up, a recipe edit could be performed (it wasn’tthe case) and the measuring data could be seen;

• The measurement was started from Start and while running, the parameters wereadjusted;


• The real peak positions were corrected to the nominal mass numbers by modifyingthe Mass Scale Offset which shifts the mass scale and the Mass Scale Slope whichshrinks and stretches the mass scale. See adjusted peaks above in Fig.2.12;

• The Stop button turned off the process, saving the project and eventually applyingit to all measurements.

2.3.6 Ion source calibration

When calibrating the ion source (grid ion source in this case), the following parametershave to be adjusted:

• The filament number – this parameter depends on the ion source type;

• The emission current – is the filament emission current;

• The protection current – is the maximum filament current, which protects thefilament;

• RF-polarity – it switches the polarity of the rod system for separating ions by them/e ratio;

• Ion reference – these are the ion source voltages;

• The cathode, focus, field axis and extraction parameters – these parameters dependon the used ion source [1].

For the PrismaPlus QMS, the parameters for the grid ion source were implemented,excepting the Polarity where a negative polarity have been found to give better definedpeaks than a positive polarity as it was suggested by the default parameters set.

Fig. 2.13: Ion source tuning with adjusted parameters


2.4 Ultraviolet radiation on Mars

In order to quantify the amount of UV radiation reaching the surface of Mars, a shortmodel describing the UV flux budget between the top of the atmosphere and the surfaceof the planet, is presented.

The solar radiation reaching the top of Mars’ atmosphere is considered to be the initialamount of radiation that one has to account for while developing a radiation flux model.It strongly depends on the areocentric longitude, Ls the latitude and the time of the day,which are the parameters required to describe the position of the Sun in the sky [22].

Following the entry in the planet’s atmosphere, the radiation is further affected by aseries of parameters, which altogether describe the atmospheric conditions. The total UVradiation reaching the surface of Mars is actually the sum of two separate components: adirect attenuated flux and a diffuse flux.

2.4.1 Solar radiation

The solar radiation consists of the energy we receive from the Sun (solar atmosphere)and it can be received as visible light, radio waves, infrared light, X-rays or ultravioletand it is the source that provides electromagnetic radiation for each of the planets ofthe Solar System. When the radiation budget of a planet has to be determined, it isessential to know the incoming radiation at the upper atmospheric level and the existentatmospheric interactions, so that it becomes possible to gain quantitative and qualitativeinterpretations of the radiation at the surface of the planet.

For Mars, it is easy to assume that the spectral composition of the Sun radiationreaching its top atmosphere is the same as for Earth, but the intensity (irradiance) differsas a function of distance.

The specific intensity Iν of the radiation at a frequency ν [Hz] is defined by:

dE = IνcosθdAdtdνdω (2.11)

where dE is the amount of energy crossing an area dA so that the irradiance is definedas the amount of energy passing through unit area (perpendicular to the beam of radiation)per unit time per unit frequency interval into unit solid angle.

The units for Iν are erg cm−2s−1sr−1Hz−1 [45].

Fig.2.14 represents the 1985 Wehrli Standard Extraterrestrial Solar IrradianceSpectrum spanning over the 199.5 and 3200 nm range (the 3200 nm limit has been


Fig. 2.14: The extraplanetary solar spectrum (Data has been taken from the Wehrli database)[35]

deliberately chosen by the author to enhance the spectrum range that is mostly relevantfor the current work).

The more recent ASTM E490 spectrum is a reference spectrum developed by using datafrom satellites, space shuttle missions, high-altitude aircraft, rocket soundings, ground-based solar telescopes and modelled spectral irradiance [35].

The mean solar irradiance given by the ASTM E490 for Mars is 588.6 W ∗m−2 , with715.9 W ∗m−2 at perihelion and 491.7 W ∗m−2 at aphelion [34].

2.4.2 The UV flux at the upper atmosphere of Mars

Important evidence of the UV spectra at the top of the Martian atmosphere wasacquired by the Mariner 6 & 7 spacecraft in 1969 and by the SPICAM ultravioletspectrometer on board of Mars Express, more recently, in 2004. Both missions focusedon determining the composition and structure of the Martian upper atmosphere, andeventually evidence on how is the spectrum varying at different altitudes and what is themechanism that produces upper atmosphere emissions has been revealed [11].

Calculating the solar flux at any point in the Martian orbit is necessary when theultraviolet flux entering the planet’s atmosphere has to be known. Increased variations ofthe solar flux are caused due to the fact that Mars presents a higher eccentricity (comparedto the Earth).

The Sun-Mars distance, r, at any point in the Martian orbit can be determined fromthe areocentric longitude by


r = d(1− e2)1 + ecos

(LS − LPS

) (2.12)

where d= mean Mars distance (1.52 AU), e = Mars eccentricity (0.0934) and LPS =longitude of perihelion (250o).

Knowing the flux at any orbital point, the input flux, F0, to the top of the atmospherecan be calculated by considering the solar zenith angle as

cos(z) = sin(θ)sin(δ) + cos(θ)cos(δ)cos(h) (2.13)

so thatsin(δ) = sin(ε)sin(Ls) (2.14)

and the hour angle h is defined as

h = 2πtp

(2.15)

introducing these parameters in

F0 = µF1.52(d2

r2

)(2.16)

where F1.52=flux at 1.52 AU, µ=cos(z), with z defined above, it yields

F0 = F1.52

[sin(θ)sin(ε)sin(Ls) + cos(θ)cos(2πt

P)×

(1− sin2(ε)sin2(Ls)

)1/2] [1 + ecos(Ls − LPs )

1− e2

]2

(2.17)This describes the top atmosphere flux for Mars when θ, Ls and t are known at any

point on the Martian orbit. [22] Fig. 2.1.5 depicts the ultraviolet spectrum plotted byusing data recorded by the Mariner 6.

Typical spectrum of the Martian disk [Image Credits: Mariner Mars- A PreliminaryReport 1969]

[11]


2.4.3 UV light in the NEW_JMMC

Fig. 2.15: Measured UV spectrum of the Xe lamp used as an ultraviolet source at theNEW_JMMC

The spectrum of the Xe arc lamp was taken by the author assisted by Magnus T.Joelsson (Chem. Dept), using an Ocean Optics Maya2000pro spectrometer. Thespectrometer measures the radiation flux in counts per integration time so it was nottrivial at all to find the photon flux emitted by arc lamp.It shows that the lamp coversentirely the ultraviolet range as on Mars although it has a higher intensity. Anotherfuture option to consider regarding irradiation with UV inside the chamber should be anLED array which emits exactly in the Martian spectrum when installed above thedetector with ca. 3cm. This device was made by Jonathan Merrison at the MarsLab inÅarhus but its insuficiency is that tends to overheat within a few minutes after it isswitched ON. A small cooling system attached to one of its sides would permit anefficient source of UV for future experiments.

2.5 The pressure and temperature at the surface of Mars

The climate of Mars is complex, implying many dynamic processes that can occurlocally or globally.

Starting with the Viking program in 1975, in situ climatic measurements started to berecorded and continued remotely from the 2001 Mars Odyssey and Mars ReconnaissanceOrbiter. Ever since, each landed mission has been observing the atmospheric dynamics ofMars in different geographical locations, providing data for further analysis.

Modelling the atmosphere behavior of the Red Planet is not a trivial task toaccomplish becaue relevant information about how the solar heating of large masses ofair, the cloud distribution or the thermal inertia of the ground influence pressure andtemperature variations, are still incomplete.


The present configuration of the simulation chamber permits only the minimum thatcan be done in terms of achieving a temperature value within the Martian range.

Fig. 2.16: Air - ground temperature variations on Mars

2.5.1 Simulated pressure inside the NEW_JMMC

The PX409 Pressure Transducer which measures gauge pressures in the vacuumrange (between 0 and -25 PSI), was used to monitorized in real-time the pressurevariations inside the NEW_JMMC. Once the appropriate pressure range is beingreached by vacuuming the enclosure where the transducer is installed, it starts displaying1 reading per second through the interface of the Omega TRH Central software.

Fig. 2.17: Photo of the PX409 Pressure Transducer taken by the author

It is quite easy to confuse negative gauge ranges with absolute pressure ranges; however,one can see the slight difference between them by knowing the reference pressure for anyof them.

Negative range pressures will always refer to pressures reported to the normalatmospheric pressure, while the absolute pressures will ignore the atmospheric pressureand measure strictly the values within a defined volume. By reading either in negativeranges or in absolute ranges, the pressure difference is basically the same but the finalmeasured values will differ due to the difference in their reference point.


The core of this device is a micro-machined silicon sensor which has a high sensitivityin terms of measuring very low pressures. The connection with the pc is directly madethrough a usb port. Having a constant image over the pressures within the chamber andtesting the dimension of the leaks going on during the testing stages, has always beenextremely important.


2.6 The cooling system of the NEW_JMMC

The development of the cooling system at the NEW_JMMC was a new idea whichappeared during the assembly process, while the author was visiting the MarsLab inÅarhus. Jonathan Merrison was the one who provided the first two Peltier elements thateventually have become part of the cooling system. He also offered very practicalsuggestions on how could such a system be implemented in an environmental chamber.

The first attempt in gaining an efficient cooling was made by constructing a stackedsystem made by attaching two Peltier elements to a heat sink. This assembly was designedby the author and later on, manufactured by the mechanical workshop engineers. Ametallic cylinder with a high of approximately 2cm and a diameter of 7cm was used as aheat sink for the system, by making full contact between the top of the cylinder and thesurfaces of the elements. However, the heat produced by the Peltiers exceeded the heatcapacitance of the metallic cylinder which got overheated and couldn’t provide a fast heattransfer to the chamber walls. Heat pipes were added to increase the heat transfer ratebut it was still insufficient to get rid of the excessive heat.

The idea was dropped and a new cooling system based on water cooling started todevelop. It was a challenge to include water cooling in the vacuum chamber but theexcellent collaboration with the mechanical workshop led to a successful development ofthe water cooling set-up.

Fig. 2.18: 1. Silver conductive paste and Epoxy glue applied on the Peltier elements; 2. Stackingof two Peltier elements; 3.Arrangement of the 2 X 2 stacked elements mounted beneaththe sample support


The Peltier effect consists in a temperature difference created when a voltage is appliedbetween two electrodes which are connected to a sample made out of a semiconductormaterial. For localized cooling of relatively small areas, this effect is very useful as it offersa rapid heat transfer towards a heat sink. The electrodes of a Peltier element present a highelectrical conductivity and the semiconductor material between the electrodes creating twojunctions between dissimilar materials, enhances the heat dissipation from one side of theelement towards the other.

Theoretically a single element can achieve a temperature difference, dT, between thehot and the cold sides of the system of ca. 60oC, however in practice it is difficult toachieve dT>40oC [5].

To enhance the temperature difference, the four elements used at the chamber havebeen stacked two by two and positioned beneath the sample holder (Fig. 2.18). Each layerincluding two Peltier elements with areas of 4 X 4 cm was placed on a copper pad whichwas subsequently attached to the sample holder. The heat sink for this entire systemconsists of a semicircular copper pipe which recirculates cold water in a single direction.Sealed feed through was constructed for the water tubes on the blind flange situated onthe back side of the chamber.

When stacking the elements, conductive silver paste obtained from the QuantumDevices Dept. was used combined with Epoxy glue to stick the elements together. Thepaste was evenly applied on the central part of one of the sides of each element becauseit offers a very high conductivity, while Epoxy glue (which gives a higher resistance) wasapplied only on the rim of the sides (Fig 2.18.a).

Fig. 2.19: Tubes and feed through of the cooling system

3Experimental set-up

3.1 The architecture of the NEW_JMMC3.1.1 Improvements brought to the old JMMC

This section briefly evaluates the improvements brought to the previous chamber inorder to upgrade it to the present NEW_JMMC equipment. The entire work carriedalong the re-building of an improved version of the former JMMC, has had as mainpurpose the elimination, for as much as possible, of the limitations encountered at theold chamber’s both design and functionality. Insufficiencies given by the lack of funds(and not ideas) required many improvisations that couldn’t guarantee accuracy andappropriate working conditions right from the start. Asmus Koefoed, and I, had torethink the entire set-up in a better shape. During the assembly, previous gaps started tobe filled in and further ideas appeared along the way.

The glove boxAdding a glove box became a need when the importance of having a minimal leakage

of air inside the NEW_JMMC has been determined. During the 2013 experiments, a dryinert atmosphere was created inside the glove box, surrounding the main structure of thechamber.

Argon has been chosen as the blanket gas for the NEW_JMMC mostly due to theprecaution taken at the workplace; even though argon has a similar asphyxiationpotential as nitrogen does, it has a slightly odor print which can be more easily detectedthan nitrogen, to which humans are accustomed. It is a non-flammable gas and createssuitable conditions for handling samples while maintaining Martian conditions. (see3.1.2 The Glove Box section)

The antechamberThe antechamber attached to the glove box facilitates the transfer into and out of the

working atmosphere without affecting the clean environment created in the glove box. Ithas an increased importance in our setup due to the fact that the user is able to transfer

Experimental set-up 39

tools, maintenance equipment or samples into the glove box at any time.

Determining the MAA purityThe Martian Analogue Atmosphere (MAA) was more ‘a difficult to control’

parameter caused by the deficiency of not having a mass spectrometer which could havehelped very easily to avoid the ‘guesswork’ which actually was the only way to settle thevalue of the MAA at the JMMC. The new Quadrupole Mass Spectrometer (QMS)achieved by the Mars Group early last year, has been the most important investmentdone throughout the building of the NEW_JMMC. (see 2.1.2 The Martian analogueatmosphere (MAA) section)

The analyzer chamberThe MAA chamber represents the container having a volume of 0.644l where the

simulated Martian atmosphere has been analyzed. It is connected to the main reactionchamber on one side and to the UHV chamber on the other, while it also shelters theQMS’s analyzer. The main function of this chamber is to receive a defined volume of theMAA after UHV has been created within it and to maintain the volume of gas while it isbeing analyzed by the mass spectrometer. This chamber should be kept closed as muchas possible to protect the QMS analyzer from contamination.

The UV sourceA xenon lamp emitting also in the UV range, has been used as a new UV radiation

source to irradiate the samples in the chamber. Covering the UV spectrum of radiationfrom Mars, the Xe lamp has been one of the most important achievements during therebuilding of the chamber.

It has a considerable disadvantage though, which is the heating it produces inside thereaction chamber. However, the cooling system implemented in the set-up meant to cooldown the samples close to Martian temperatures, has also helped to prevent theoverheating of the sample support.

Cooling the TMPIn 2011, one of the advantages of the JMMC was its mobility and flexibility to be

moved around as desired; thus, a minimal set of connections to the surrounding area wasmade. The Zalman Reserator used for cooling the turbomolecular pump encouraged themobility of the assembly by avoiding its connection to the local water supply. However,the lack of a good insulation of the conducting water tubes and the reduced flow neededan improvement, in order to have the best working conditions.

On the other hand, the fact that the heavy glove box which now holds theNEW_JMMC is far from being able to be moved back and forth, encouraged the idea ofa direct connection of the TMP to the water supply of the building. With an increasedwater flow and a lower water temperature, the cooling of the TMP has been done moreeffectively.

Cooling the sample supportThe sample support was entirely built by the NBI workshop and went through multiple

stages until it reached its final design. The cold finger planned to be used in order to gain alittle bit of cooling under the chamber, became way to small and inefficient to produce evena slight cooling of the simulated environment. Two Peltier elements have been receivedfrom the Åarhus Mars Group and the idea of local cooling of the sample appeared. Initially,


the elements were mounted on a relatively big piece of metal which was meant to absorbthe heating produced through the Peltier effect; apparently, the heating was too intensiveand the system had to be rethought. Eventually, two more Peltier elements have beenbought and a water cooled copper plate has been attached to the 2x2 system of Peltierelements.

At the beginning, the idea of water cooling inside a vacuum chamber seemed a realchallenge, but a very efficient work done by the mechanics from the workshop broughtthe idea to live.

The cold fingerThe cold finger installed below the sample support, was connected to one of the

chamber’s small flanges. It is actually made of a Peltier element mounted on a pc coolingfan which acts as a heat sink. Even though its contribution to the cooling of the samplearea is minimal, it cools down mainly the left and bottom sides of the reaction chamberwhich simultaneously are heated by the xenon lamp. The cold finger can also help toaccelerate the condensation rate of the present residual water molecules.

Monitoring the pressure inside the chamberThe pressure inside the chamber was constantly monitored via the pressure

transducer attached to the NEW_JMMC. By measuring absolute pressures, it waspossible to see at any moment how the pressure was droping or increasing (when pumpswere stopped and leaks occured). The user-friendly interface provided by the OMEGATRH Central was a helpful tool during measurements, by creating charts and real timedata output.

Easy access to the chamberThe access into the chamber has been done through the front side of the main

chamber where a manually actuated VAT valve was mounted. This turned out to be themost effective and safe way to get the samples in and out of the chamber without havingto unscrew bolts during the experiment or to rely on the pressure difference between thedepressurized chamber and the pressure inside the glove box which would have kept ablind flange tightly attached to the chamber.

Carbon dioxide injectionAt the JMMC, the MAA was created by using sublimating dry ice pellets. The new

method of injecting CO2 has been done by directly connecting a 20 l CO2 cylinder to thechamber, controlled through a tap valve. Thus, the gas access has become more easy tohandle and to control.

Neutral density filtersTwo neutral density filters with optical depths of σ=0.6 and 1.3 respectively, have been

bought in order to simulate different Martian atmospheric conditions. It is possible to usethe filters independently or supperposing them and gaining thus a σ=1.9 optical depth.They can easily be placed inside the filter holder mounted on the sample tray.


3.1.2 The Glove Box

Building-up and working with an environmental chamber usually requires awell-designed and highly sealed area which can provide, on one hand a clean inertatmosphere and on the other hand, a high accessibility and manipulation of theexperimental equipment. (see also Apendix C - Glove box features)

A glove box meets up such requirements and offers a suitable option to be considered,when it comes to efficiently construct and handle an environmental chamber. The need fora glove box has arisen mostly due to the fact that the container used previously as a glovebox was the main cause of the gas leaks which considerably affected the measurementsand consequently led to unsatisfactory results.

The glove box that our group has achieved is a Labstar Glovebox workstationmanufactured by mBraun in Germany in ’94. It previously belonged to the ChemistryDepartment at HCØ Institute, University of Copenhagen. Asmus Koefoed requested theglove box workstation from the department and within a few weeks it has beentransported by specialized technicians, from the second floor of the Institute to thebasement. It was mounted on a leveled floor, with a clearance from the walls of cca 40cm, leaving enough space to access the main parts of the glove box. The environmentaltemperature of cca 20-22oC felt into the temperature range recommended for a goodfunctionality of the glove box which is between 15-30oC.

Fig. 3.1: Moving of the glove box from the Chemistry Department to the Mössbauer Laboratory


3.1.3 Inert gas purification and regeneration system

The role of an inert purification system is basically to remove oxygen (O2) andmoisture (H2O) from a given volume of air, up to a purity level of less than 1 ppm, asthe abundance of these molecules increases the risk of undesired dangerous chemicalreactions with reactive materials used in research.

Gathered into a very complex system, the components of a purifier usually are: acirculation blower, a copper catalyst, a molecular sieve, a vacuum pump, a pressurecontroller, a regeneration controller, a footswitch, isolation valves, solvent removalsystems and exhaust traps. In a purification process oxygen and water molecules aretrapped by, and then removed from the regeneration gas by two separate agents. Amolecular sieve filters the water molecules out through molecular adsorption, while theoxygen molecules are captured by an oxygen reactant material, which generally is finelydivided copper on an alumina matrix.

Fig. 3.2: Structure of alumino-silicates formed by corner-sharing of SiO4 and AlO4 tetrahedraImage Credits: Max Planck-Institut fur Kohlenforschung: Functional Materials - Zeolitesand Related Molecular Sieves

Molecular sieves are high porous synthetic alumino-silicates (Fig. 3.2) that canadsorb molecules from gases or liquids small enough to enter their pores. The forcesinvolved in the adsorption are Van der Waals forces [8]. When oxygen is filtered by thecopper sieve, they instantly react, forming copper oxide, as shown below.

Cu(s) + 12O2(g) → CuOs (3.1)

In order to have a cyclic purification process, the oxygen and water molecules have tobe removed from the sieves they were trapped in. Water is vaporized by a heater includedin the purifier and then carried out of the system by a dry gas, while a hydrogen rich gas(which is the regeneration gas) flows through the copper reactant, forming metallic Cuand water; the water is then pumped out.

The purifier of a glove box is relatively sensitive to chemicals that form more stablecompounds than copper oxide after reacting with copper. Halogens, alcohols, sulfates or


mercury vapors are some of the compounds that would require the installation ofadditional traps in order to protect the purifier.

3.1.4 Creating an inert atmosphere

As it happened to our glove box as well, the O2 and H2O levels can only reach normalatmospheric values because the source gas is surrounding air. The purifier system decreasesthese levels down to less than 1ppm and keeps their value constant up to the point whentransfers are done between the glove box and the external environment. This is when themoisture and oxygen levels are affected and the system has to pump in working gas inorder to restore them.

Two separate gases are required to purify the glove box. The inert gas used in thepresent set-up was argon, supplied by a 20l cylindrical container having its own flowregulator and being connected through the working gas pipe to the glove box purgingsystem. The regeneration gas has to be a mixture of H2 and argon if Ar is used as aworking gas. The mixture has to contain 95% argon and 5% hydrogen.

For further development of the measurements done within the glove box, it isrecommended that the moisture and oxygen probes respectively, to be cleaned and testedin order to gain a more detailed insight over the moisture and oxygen levels.

However, during the measurements and experiment conducted at the NEW_JMMC,the operation panel COROS OP 15 failed to work properly, so the inert atmosphere wascreated manually by purging the glove box (see subsection 3.2.3 Purging the glove box)

3.1.5 The oxygen and moisture probes

The mBraun workstation is equipped with a moisture probe and an oxygen probe(moisture and oxygen concentration analyzers).

The measuring principle of the moisture probe MB-MO-SE1 is based on the moistureabsorption in a thin layer of phosphoric acid (in its dehydrated form) that is coated on thesurface of an insulator between two platinum wires, and the electrolysis of the resultingH+ and OH− ions to H2 and O2 [42]. What happens inside the probe is that the sensorintercepts the concentration of the water molecules which increase the conductivity of thephosphoric acid, by measuring the current left after the molecules have been removed.

Although, the probe comes calibrated for zero-signal, span and temperaturecompensation, it is recommended that calibrations to be done annually with calibrationgas. Also, the surface of the sensor has to be cleaned at least once every 3 months. Theprobe removal instructions can be found in the Technical Documentation for MoistureProbe MB-MO-SE1 from mBraun [42].


The oxygen probe MB OX-SE-1 is able to detect the amount of residual oxygen fromthe glove box within a range of 0-1000 ppm of oxygen. It is a combination of a sensor andelectronics, where the sensor-head is protected from external mechanical effects by meansof a screw cap and the sensor element is a miniaturized Zirconium Dioxide plate which isoperated at high temperatures and is controlled by a platinum resistor [43].

As the oxygen probe has to be calibrated at least once a year, it is understandablethat our glove box probes request new calibrations before usage.

Fig. 3.3: Picture of the oxygen and moisture probes

3.1.6 The antechamber

Attached to the glove box is a large cylindrical antechamber provided with a stainlesssteel sliding tray.

It is directly connected to the glove box’s vacuum pump and can hold a depressurizationof up to -1.0 bar. Two steel doors that can open upwards, close the antechamber at bothends. When vacuum is created inside the antechamber, the doors are protecting the volumethrough a very good sealing.

Usually, the antechamber is used to transfer tools or samples inside the glove boxwithout affecting the clean inert atmosphere. However, several times during the buildingof the NEW_JMMC, the antechamber was used to speed up the drying of different objectsplaced inside, or to remove gas molecules trapped in the Epoxy glue used to stack thePeltier elements together, allowing thus a much stronger adhesion between them.


Fig. 3.4: Pressure drop inside the antechamber

3.1.7 Other specifications of the glove box

The glove box is made out of stainless steel and has 2 DN40KF electricalfeedthroughs included. Other two holes have been drilled in the back wall in order to fitthe supplementary vacuum pump, water and electrical connections. The initialfeedthroughs have been highly sealed but for the new holes silicon sealant was applied inorder to fill the empty spaces between the tubes.

The glove box is also provided with a box filter on the internal wall, having a depositiongrade of 0,3µm. A scratch resistant polycarbonate window represents the front wall of theglove box. The window carries the 220mm diameter glove ports where the newly orderedneoprene dry-box gloves have been attached to.

The adjustable stainless steel shelf has been used to sustain the QMS and the analyzerchamber; it also holds the electric outlets. During the arrangements of the NEW_JMMCthe shelf has been rotated upside down so that a little bit of extra space was gained.


3.1.8 The main chamber

The reaction chamber is actually an LF 8-way cross with 3 LF160 tubes, 1 LF80 tubeand 4 DN40KF tube. It is made out of stainless steel and has a volume of 12.82 l ( seeAppendix A - Volume of the main chamber). The size was found to allow a proper fittingof the sample support, cooling system and the electric wires without congesting any ofthem.

The 8-way cross has been attached to the other parts of the NEW_ JMMC throughsuitable centering rings which align and support the VITON O-rings and which havebeen fastened to compress the seal between the flanges using either hinged clamps, bandclamps, single claw clamps or double sliding claw clamps.

Fig. 3.5: LF 8-way cross as main reaction chamber (center), blank flange, centering and O-rings,hinged clamps, band clamp, single claw clamps and double sliding claw clamps

In terms of overheating, there is a slight chance for the main chamber to get very warm.The main heating is produced by the Xe lamp which even though is not negligible, it doesnot cause a major concern; first of all for such a heating source the heat storage capacityof the 8-way cross is relatively large and secondly, cooling sources are also present i.e. thecold finger at the bottom of the chamber, the cooling system of the sample holder and theTMP cooling system.


3.1.9 Volume of the main chamber

Finding the volume of the main reaction chamber required more than metricmeasurements because it contains the sample support and the electrical and waterconnections, so all those should have been subtracted from the total volume of thechamber. Similar calculation as done for the UHV and the analyzer chambers (which forthe main chamber would have been much more complicated to do because of its complexgeometry) or the more traditional way of calculating the volume by filling it with water,were eliminated from the start; instead, the volume has been found as it is describedbelow.

An ISO T piece was connected to the upper inlet of the chamber in order to permit thedouble connection of the PX 409 pressure transducer and of an additional volume to it; asan additional volume, the Cole Parmer vacuum oven existent in the lab was used because ithas a very well defined volume and its gas volume can to be easily connected/disconnectedfrom a system.

Notes: 1. During the measurements, the solanoid valves 1 and 2 were permanentlyclosed in order to avoid any gas exchange with the analyzer chamber.

2. The TMP wasn’t used during these measurements.3. The volume of the oven was calculated beforehand to be 18.75 l

Fig. 3.6: Photo of the main chamber- oven system

The chamber has been directly connected to the oven through a sillicon tube (Fig.3.6) and the ON/OFF switch of the oven represented the only delimitation between thetwo volumes. The procedure by which the volume has been determined was repeatedthree times for more accuracy of the results, as it follows:


• The procedure started with the VAT valve opened and the oven’s gas inlet switchedON (equal pressure in the coupled system).

• With the VAT valve opened, the BP was ran until a pressure of aprox. 30 mbar wasreached; then the BP was closed, letting the pressure inside the system to stabilize.

• Air was slowly let into the system through the needle valve 2 until the system’spressure increased to aprox. 100 mbar (value chosen for ease of calculation); at thispoint the oven inlet was closed (so that poven=100 mbar).

• The BP valve was opened and the main chamber solely was vacuumed again untilaprox. 0 mbar (pchamber=0 mbar).

• At this point the VAT valve was closed down so that the only additional volumebetween the oven and the chamber was the sillicon tube connecting them.

• The oven inlet was opened and the pressure was let to stabilize resulting peq.

By using the ideal gas law, the volume of the main chamber has been deduced, asshown below:

pV = nRT (3.2)

pchamberVchamber = n1RT (3.3)

povenVoven = n2RT (3.4)

peq(Vchamber + Voven) = (n1 + n2)RT (3.5)

(3.3), (3.4), (3.5) => V1 = pchamberV2 − peqV2peq − pchamber

(3.6)

finding out the capacity of 12.82 l of the main reaction chamber.


3.1.10 The vacuum system

Creating an environmental chamber requires an efficient vacuum system able to removeatmospheric gases in order to enter the desired mixture of gases. The first step afterbuilding up the NEW_JMMC as a highly sealed tank, was to obtain, control and maintainvacuum as long as it is needed.

The present set-up benefits of a vacuum system consisting of a turbomolecular pumpsustained by a back pump. This coupling is often used when high vacuum is to becreated; the back pump creates a partial vacuum required for proper working conditionsof the turbomolecular pump.

3.1.11 The Back Pump

The back pump used at the NEW_JMMC is a Pfeiffer Balzer DUO 016B, also used atthe old JMMC. It creates a partial pressure by removing gas molecules and within aprox.30s assures the optimal low-pressure required to start the turbomolecular pump.

Fig. 3.7: Architecture of the back pump


The BP can be switched on/off in any pressure range and has the maximum exhaustpressure at 1.5 bar. The lowest run-up temperature is +12oC, the nominal volume flowrate works at 50/60 Hz and it has a value of 16.2 m3/h. The exhaust connection is madethrough a DN25KF flange so it can be easily connected to the glove box. The operatingmedium P3 oil is distinguished by its low vapor pressure, good lubricating action, favorablealkaline reserve and high oxidation resistivity.

The pump has to be placed on an even, flat surface, the maximum ambient temperaturehas to be +40oC and an adequate air circulation has to be provided [47].

The main parts of the BP used at the NEW_JMMC are depicted in Fig. 3.7.The operating medium has been changed during the preliminary tests, run with the

BP, and the replacement procedure is described under the 3.3.2 Changing the oil of theback pump section.

Fig. 3.8: 1. Back pump pressure drop; 2. Back pump pressure drop zoomed in around p=0

3.1.12 The Turbomolecular Pump

The core of the vacuum system is the turbomolecular pump which is the most importantand dangerous component of the entire assembly, if not operated correctly. It is a PfeifferBalzers TPH-240 Turbo Molecular High Vacuum Pump with a designated speed of 240L/s[32].

Its inlet flange is a LF 100 which has been directly connected to the UHV chamber,without using other converter flanges. The outlet flange is a KF25 and has been connectedthrough the VAT valve 3 to the main exhaust line.

The complexity of such a pump is high and that demands very careful handling andcontinuous water cooling while in function. The operating principle is based on creatingan oriented flow of the molecules towards the exhaust, in order to create or to maintain acertain level of vacuum. Most turbomolecular pumps employ multiple stages consisting ofrotor/stator pairs mounted in series. Gas captured by the upper stages is pushed into thelower stages and successively compressed to the level of the backing pump pressure. The45o tilted blades of the rotor hit the molecules, giving them an unidirectional motion.


The high rotor speed implies a mandatory cooling system. This is provided throughdirect connection to the local cold water supply. The two water connections (recently fixedat the workshop) of the turbomolecular pump allow a constant flow of the cold water andtherefore avoid the overheating of the pump. It is very important that the cold water to beswitched off when the pump is not in use because over longer periods of time, condensationoccurs around the TMP and water can drip into the electrical connection (see the 3.3.1Workplace hazards section).

The pump is controlled via a TPC-110 turbo controller which can be very easilymanipulated with an on/off switch.

Fig. 3.9: TMP pressure drop

3.1.13 The support of the chamber

Fixing the entire set-up on supports took relatively a long period of time because itwas quite tricky to find the appropriate parts to sustain the whole construction. Thesophisticated geometry but also the increased weight of the NEW_JMMC requested along seeking time before the present feet has been ready to hold everything up.

Two individual steel feet have been found in the spare parts deposit at the HCØInstitute, and on the tip of each foor a plate was fixed in order to have a larger area wherethe pressure exerted by the NEW_JMMC to be equally distributed.

Mounting the supports was again a ‘heavy’ task to complete, when the set-up had tobe lifted many times before everything was evenly aligned. A hydraulic crane with 2 tonlifting capacity was used several times, when hand power was way to weak to help.


3.1.14 The sample support

The sample support has been entirely designed by the author and manufacturedafterwards in the mechanical workshop at the Niels Bohr Institute. It was designed insuch a manner to fit the interior of the main chamber, with two curved plates assupporting feet, created in a way that a good fixation can done between the support andthe curvature of the 8-way cross.

There is also the sample tray which fits perfectly the support and can be moved backand forth easily. It is provided with the filter holder where the neutral density filters canbe placed. These filters were not used for the preliminary experiments but it is possibleto fix them in the support whenever it is needed.

The support itself is fixed by screws at both ends which permit a rotation of thesupport to almost any angle. This is convenient in situations when the samples situatedon the sample tray have to be positioned on different angles (Fig. 3.10 and Fig. 4.3).

Fig. 3.10: Fig. 1 and 2 - the sample holder in upright position and tilted position, respectively;Fig. 3 - sample holder tray with the attached filter holder


3.2 Operating procedures3.2.1 Operating the valves

Fig. 3.11: Set-up of the NEW_JMMC

Fig. 3.11 depicts the main compartments of the NEW_JMMC and the valves whichcontrol the access from one compartment to another or to the vacuum pumps. The roleof each valve and the order in which they have to be operated has a major importance inassuring a safe manipulation of the NEW_JMMC and in obtaining an increasedperformance of the entire system.

During the operation of the vacuum pumps, high pressure differences can arise betweentwo or more different compartments of the set-up, so that the valves must be carefullyoperated in order to avoid any damages of the assembly or more important, to eliminatepossible injuries of the operating personnel.

In the followings, each individual valve will be described, while its linkage to the restof the set-up can be sensed in Fig. 3.11; they are described in a random order, regardlessof their function or importance.

Note: When NEW_JMMC is mentioned, it refers to the entire volume of the set-up


i.e. the Main Chamber + the Analyzer Chamber + the UHV Chamber and the VAT valve1 is considered to be open. Otherwise, each individual chamber in question will beseparately denominated.

• Needle valve 1 is used to equalize the pressures between the surrounding atmosphereand the interior of the NEW_JMMC. Because it can be loosened step-by-step, itcomes easy to handle it, while the inflow of the surrounding gas can also be controlled.

• Needle valve 2 can be unscrewed every time when a pressure equilibrium is neededaround VAT valve 1; this usually happens when the pressure difference increasesbetween the two sides of the VAT so that it cannot (and is strictly forbidden to) beopened as it can easily be destroyed. However, needle valve 2 can do the same jobas needle valve 1, and that is to release the surrounding gas into the NEW_JMMC,equalizing the pressures.

• The CO_2 tap valve is an On/Off valve and controls the inflow of the CO2 into themain reaction chamber.

• VAT valve 1 is situated between the UHV chamber and the main reaction chamberand has a very important role in terms of separating the two volumes wheneverpressure differences have to be acquired or analysis of the gas composition insidethe main chamber needs to be done. The VAT valve originates from Risø and ispneumatically operated by means of a control box which closes the valve if power islost [32].

• VAT valve 2 is a manually actuated valve and it was bought from the spare partsdeposit of the HCØ Institute. The main reason for its acquisition was the need of aneasy-to-manipulate gate towards the reaction chamber which would assure a quickaccess into the chamber but in the same time could guarantee an excellent sealingwhen vacuum is created inside. The valve is simply actuated by a vertical handlerdirectly connected to the valve’s gate and which permits only two positions, ON andOFF.When opened, the sliding tray of the sample support can be pulled out through thevalve just enough for the user to be able to place the samples on the desired spot.Besides the VAT valve 2, a blind flange could have been used as an access port butclamping it down with screwed-clamps would have taken considerably longer time.Relying only on the suction created by the vacuum to firmly attach the flange to thechamber, could have been quite dangerous to operate.

• VAT valve 3 is a small manually actuated valve situated behind the TMP, on thevacuum line towards the BP. When leaving this valve open, the NEW_JMMC isdirectly connected to the pump’s suction which would be able to tightly attach forexample a blind flange to the chamber.Whenever vacuum has to be held inside the chamber while the pumps are stopped,it is a good idea to close VAT valve 3 and thus avoid further leaks from the vacuumline to add up and increase the pressure inside the chamber.


3.2.2 Operating conditions

Before starting to simulate a desired environment inside the NEW_JMMC, the usermust always ensure that:

1. The glove box is completely sealed down and the connection to the purging gas(argon) is correctly done.

2. The antechamber doors are completely closed down.

3. The main water supply delivering the required quantities of water towards the TMPand the cooling system is switched ON.

4. Each valve which in the ON position create a direct access between the chamber andthe glove box is turned OFF; otherwise, the suction of the vacuum pump will draginto the chamber a considerably high volume of Argon and by all means that has tobe avoided.

5. The nitrogen main supply feeding the VAT valve 1 is ON, so that the valve can beautomatically opened or closed through the attached controller box.

6. The glove box and the entire working space is properly illuminated as long as theworking procedures are executed, and preferably also while the experiments arerunning.

3.2.3 Purging the glove box

The main purpose of the glove box was to maintain an oxygen-free environment,necessary to cleave and handle the olivine without oxygen reacting with its surface.

The ambient air had to be replaced in the glove box in order to obtain a purenitrogen/argon atmosphere. The inert atmosphere has been created neither through thepurification nor the recirculation processes but manually, by purging the volume.Displacing the ambient air from the system is called purging. Working gas, in this casenitrogen and argon, is used as purging gas [40].

An inert atmosphere is considered to exist in the glove box when the O2 level < 250ppm is indicated by the control panel. Usually, the purging is going on until the value ofO2 decreases.

The control panel of THE glove box hasn’t been correctly functioning all this time, soinstead of purging the glove box once, it was done five times to compensate the lack ofelectronic displaying and make sure the O2 level has been truly decreased. The processwas repeated three times with dry nitrogen and two times with argon.


To fill up the glove box manually required a tube inserted through one of the glovebox’s blind flanges with a bit of space left besides the tube, through where the air andexcess purge gas would be pushed out.

Fig. 3.12: Ping pong ball gas flow meter showingthe volume/time ratio of nitrogenentering the GB

The argon cylinder is provided witha gas flow meter which made it easierto control the gas volume entering theglove box; however, the nitrogen wasdirectly injected from the local supplyso that a ping pong ball flow meter,installed on the nitrogen line, was used.

After each round of purging,the glove box was closed down andleft still for aproximately 20 minutes.When the 5th round was completedthe glove box was considered to have aminimum amount of O2. The durationof a complete round of purgingwas found as it is described below.

Calculating the required quantity of gas necessary to purge the GB once

boxvolume[m3] · 5.000 = purginggas[liters] (3.7)

which resulted in a required quantity of gas of 3,975 l

Ping pong ball gas flow meter

The graded ping pong ball flow meter (Fig. 3.12) regulates the gas flowing through it.It is graded from 0 to 6 with 0.5 steps and each step represents the volume of gas passingthrough the flow meter. The level is indicated by the bottom of the ball that floats drivenby the volume/time ratio of the gas.

Therefore, the nitrogen flow was regulated such as the ball indicated the value 5,meaning a rate of 5 m3/h ; so knowing that 0,795 m3 of nitrogen/argon was needed forpurging the GB once, the time for this to happened was calculated to be between 9-10minutes [41].

3.2.4 High vacuum creation procedure

The first stage of any experiment conducted in the NEW_JMMC must focus on the’cleaning’ of the chamber by intensively removing the residual gases from inside. Thisprocess can take between 45min and several hours depending on the time allowed to


this operation but on average approximately 2-3 hours of decontamination should givesatisfactory results.

The argon shield that creates an inert atmosphere around the set-up, protects the cleanatmosphere of the chamber against possible contamination from outside; therefore, it ismore convenient to open the chamber for insertion of samples or for short maintenanceworks without compromising the clean environment from inside. It is obvious that furthervacuuming will be needed once the chamber is closed again but argon is far from being sosticky and tend to linger as much as e.g. water molecules would do.

As by the 2013 configuration of the installation (Fig. 3.11), the following procedurehas been performed to gradually clean the chamber:

1. VAT valve 1, VAT valve 2, valves 1 and 2 were all opened.

2. BP was started and after approximately 30 sec. the TMP was started as well.

3. Following the values transmitted by the pressure transducer, when the maximumvacuum value of aprox. -0.65 mbar was reached, the VAT valve 1 was closed.

4. The Xe lamp was switched on for about 40-45 minutes. The high energetic radiationof the lamp (mostly what is below 200nm) initiates the photodisociation of the watermolecules which enhances the outgassing of the chamber’s walls.

5. Meanwhile, spectra were continuously taken by the QMS.

Note: the reason why the VAT valve 1 was closed prior to switching on the Xe lamp,concerns the safety of the TMP, which could be seriously damaged if perhaps the suddenshinning of the lamp would splinter the viewport and compromise the vacuum quality.

The procedure was reversed in order to finish the cleaning of the chamber, as it follows:

1. The Xe lamp was switched off;

2. the QMS was disconnected;

3. VAT valve 1 was opened;

4. TMP and BP were stopped;

5. The TMP was let to completely spin down before any gas was let inside the chamber;

6. Before opening the chamber, surrounding gas could slowly let in by unscrewing eitherneedle valve 1 or needle valve 2;

When CO2 had to be injected into the reaction chamber, stage I was completed,whereupon valve 2 was closed while the tap valve slowly let CO2 inside:

1. CO2 was injected up to a pressure of 20-25mbar;

2. valve 1 was closed and then valve 2 was opened letting a very small amount of CO2into the analyzer chamber where the QMS should detect it;

3. if experiments were conducted with CO2 inside, then the pressure was maintainedaround the above mentioned value;

4. ending the process required the same steps as for stage II.


3.2.5 Helium leak detection

The NEW_JMMC is far from being an ideally sealed volume due to the leaksoccurring at various junction points around the flange fitting, electrical or water feedthrough. Scratches or other types of damages found on the connecting surfaces of thespare parts used in the assembly can permit substantial leaks, which eventually alter thequality of the vacuum inside the chamber.

Having leaks around the set-up isn’t something unexpected and there are not manythings that can be done in order to avoid them. Therefore, the idea of shielding thechamber with an inert gas will not eliminate or minimize the leaks going on, but willminimize the alteration of the vacuum by entering i.e. Argon instead of air.

As a quick check-up (without the He spray test), the Edwards Spectron 3000S LeakDetector with the Edwards Spectron 3200 Remote Box was used to determine the levelof leakage of the system. The leak detector has a build-in diffusion pump to producehigh vacuum and a liquid nitrogen cold trap. The cold trap has a twofold purpose: first,to effectively condensate the minor amount of water from the vacuum system, andsecondly, to stop the back streaming of oil vapor from the diffusion pump to the leakdetection cell [2].

The operation procedure of the detector is as it follows:

1. The detector is switched on and the messages ”close down” and ”finish” appear onthe display;

2. The detector’s hose is connected to one of the available flanges of the chamber; thiswill be the vacuum line; the ‘’start-up” message will appear and after 1 min. the”pumpdown” message will be displayed – this is when the back pump start to createvacuum;

3. At the point when ”standby” is displayed, the detector is supplied with liquidnitrogen (up to 2.8 l);

4. The ”finish” button is pressed so that the ”finish” message will be displayed, followedby ”filament warm-up”. When the detector is ready to test the system for leaks, the”ready to test ”message” appears;

5. The system is being pumped down and the leakage rate is indicated through massive,gross, or fine. For the NEW_JMMC, the massive level has been displayed with aleak rate of 0.05 −3 mbar/sec;

6. When the ”finish” button is pressed down, the leak detection is stopped and thedetector is ready for a new test;

7. The detector is shutting down after aprox. 10 min. after the ”close down” button ispressed down.


3.3 Workplace safety and maintenance3.3.1 Workplace hazards

Fig. 3.13: Warning symbols of hazards likely to occur in the lab

• Inhalation of hazardous chemicals

Toxic materials that can enter in the human body via inhalation are usually gases,vapors and dust.The respiratory system is the fastest transporter of poisonous chemicals towards thelungs and further on, into the circulatory system, from where they get absorbed bythe entire organism. These chemicals are more or less soluble in water and the levelof solubility determines where and how fast are they absorbed by the human body.For example, the isopropyl alcohol used for degreasing and cleaning the componentparts of the environmental chamber, is highly miscible (soluble) in water, thereforethe released vapors are dissolved predominantly in the nose or trachea and areunlikely to reach the lungs in high quantities. On the other hand, the ozoneresulted from the Xe lamp interaction with the oxygen from the surroundingatmosphere, is one of the reactive gases with very low solubility in water that maketheir way until the lungs.In order to avoid ozone to expand into the working place, the Xe lamp has beenoperated mostly while the glove box was closed down. Before removing the frontwindow of the glove box, only the gloves were removed so that the ozone came outgradually and the area was left for a few minutes, while a fan was ventilating theroom.The BP is fueled by an organic operating fluid (P3 medium). Inhalation of the oilvapors or direct contact with the skin has to be avoided, especially during the oilreplacement process. When the BP is in operation, the oil gets warmed up and theexhaust filter emits poisonous vapors that by all means have to be conductedtowards the ventilation network of the building as they are damaging to therespiratory system.


• Water-cooled equipment

Fig. 3.14: Condensation on the surface of the TMP

The HCØ Institute has a refrigerated recirculator which provides cold water withtemperatures just above the freezing point for the laboratory equipment. Due tothe very low temperature of the water, condensation often occurs when the water ispassing through relatively warmer regions.This happens at the turbomolecular pump whenever it isn’t running and the watersupply has not been switched off from the wall tap (Fig. 3.14); it can be dangerous,knowing that the water will drip in the vicinity of the TMP’S electricalfeedthrough so the wise thing to do is to switch off the water tap right after theTMP has stopped.

• Using electrically powered equipment

The need of electricity can hardly be avoided in modern experimental work. Whetherit comes about powering a light source, a computer or supplying with electricity aturbomolecular pump, electric current is almost always a need. Needless to say, anydevice running on electricity presents a risk to some extent.There is an extended awareness about the precaution that must be taken whileworking with high voltages. Usually the correct handling of the working equipmentis not sufficient and maintenance check-ups should be regularly done to preventelectrocution, overheating or shorts.The provided maximum voltage at the lab is 230V and generally, the set-upcomponents were powered at 220V. The glove box is provided with a five outletsurgeprotector/power strip and the laboratory outlets are all grounded.


• Vacuum pumps

When working with vacuum pumps, there are a few possible risks that must betaken into consideration and prevention of each of them is a necessity. Related tolow pressure generation are mechanical hazards, chemical hazards or fire hazards.The back pump and turbomolecular pump have complex structures and theirbuilding parts can fail to work properly at any moment. Mechanical hazards canrarely be anticipated, therefore caution should be taken when placing the pumps inthe working area; they have to be well fitted, correctly connected to the powersupply and by all means, especially at the TMP, infiltration of external particleshave to be avoided in the vicinity of the rotating blades. Even the refilling of thechamber with surrounding atmosphere has to be done gradually after the turbineand the stator blades did spin down, as a sudden injection of air molecules couldseriously damage them and even cause an explosion.The creation of vacuum means great pressures exerting on the walls of thedepressurized volume. Great pressures equal great forces pressing upon relativelysmall areas, meaning that everything (including body parts, skin etc.) that getstrapped between a blind flange and the chamber while this is vacuumed out, willsuffer injuries.More about chemical hazards can be said when referring to the back pump and themedium used to fuel its engine. The P3 medium (oil filling the pump) has to bekept out of any interaction with other chemicals. Even the water accumulated overa relatively long period of time as a result of many hours of pumping, is altering itsquality. While working at the NEW_JMMC, an unusual overheating of the pumpwas observed and it was immediately concluded that the old oil had to be disposedand changed with new and clean one.Fire hazards can occur while working at the vacuum pumps mostly because ofoverheating during their operation. In order to prevent that, the TB has beenprovided with a connection to the local cold water supply, while the BP isbacked-up by a fan.

• Ultraviolet radiation hazards

We receive ultraviolet radiaton from the sun on a daily basis. However, this radiationhas a non-ionizing nature and in small doses it cannnot be considered dangerous.The xenon arc lamp used during the experiments at the NEW_JMMC irradiatesalso in the harmful ultraviolet range of radiation with wavelengths below 380nm,besides the visible and infrared ranges.The high frequency ultraviolet light is very dangerous for the eyes and skin and it canlead to serious eye damages or frequently, even to blindness and serious skin burns.Protective eyewear must be used during the operation of the lamp even though theuser is not directly looking to the source. The UVEX protection glasses found inthe lab have been retested before the most recent UV measurements to confirm theirshielding capacity. Direct skin interaction with the radiation should be avoided byall means.


The small gaps between the Xe lamp (Fig. 3.15) and the chamber’s viewport havebeen covered by placing a narrow sheet of aluminum foil which stops the harmfullight escaping and it will not become overheated by te lamp.Ultraviolet is also hazardous in terms of ozone creation (see Inhalation ofhazardous chemicals).

Fig. 3.15: Picture of the Xe arc lamp

• Compressed gas cylinders

Compressed gases such as argon and carbon dioxide bottles have been used whileoperating the glove box and the NEW_JMMC. These gases can be hazardous inmultiple ways: firstly, they can be the source of reactivity with other gases or cancause intoxication if released in high concentrations.Secondly, asphyxiation can occur if there is a high concentration leakage of thesegases. Asphyxiation happens not necessarily because of the toxicity of a gas butbecause of its large volume released in the surrounding area which displaces theoxygen.Thirdly, large compression pressures mean extreme forces applied upon the structureof the bottle which can be physically damaged by ruptures around the valve. Thisis why any gas cylinder should be tightly chained to the walls or fixed structures inorder to maintain it in an upright position and prevent sudden overturning.The cylinders containing argon and carbon dioxide were tightly linked to the glovebox’s feet.


3.3.2 Changing the oil of the back pump

The organic operating medium (P3 medium) existent in the back pump chamber hadto be changed while setting up the NEW_JMMC.

It was obvious that the oil had a high degree of deterioration only by seeing it veryunclear and unusually viscous. The pump was also getting overheated after being used fora couple of minutes.

The oil changing procedure is described below:

1. the solenoid valve connecting the pump to the NEW_JMMC was closed;

2. the drain screw was unscrewed and the oil was drained off;

3. after most of the oil was drained off the pump was started for 1-2 minutes toaccelerate the removal of the remaining oil;

4. the replacing procedure started by letting in only a small quantity (aprox. 100ml)of clean oil;

5. the pump was started again for aprox. 5 minutes, while the gas ballast valve wasclosed (ballast valve in position 0); meanwhile, the pump was tilted so that theold+new oil mixture could be evacuated;

6. with the pump still hot, it was refilled with 2.4l of clean oil;

7. the pump was started for about 30 minutes with the ballast valve open (ballast valvein position I);

8. finally, the ballast valve was closed and the pump ready to function properly.

As an important remark, it is recommended that the back pump operating medium to bechanged once a year, to provide appropriate working conditions of the pump.

Observations regarding possible hazards related to P3 medium handling can be foundunder the previous section 3.3.1 Workplace hazards.

3.3.3 Maintenance

Basic maintenance should be carried out at the NEW_JMMC when experiments areconducted, but also when it is not in use. The maintenance should be mostly based onkeeping clean both the interior and exterior of the glove box (including antechamber). Itmeans that contaminants of any kind have to be removed by wiping the surfaces withdistillated water or other cleaning agents.


The main components of the NEW_JMMC, including fittings and flanges, have beenall cleaned with isopropyl alcohol prior to be assembled, in order to remove grease and oilsfrom their surfaces. Isopropyl is widely used as a cleaning agent, especially for dissolvingoils, because it has a low toxicity and it evaporates rapidly.

Demineralized water has also been used to clean the exterior surfaces of the chamberbecause it has the advantage over regular tap water of having a high purity(decontaminated water) and therefore does not leave residues as it evaporates.

During the installation of the QMS analyzer and sample holder, latex gloves have beenused to avoid any further grease from the hands.

4Preliminary results

4.1 The olivine experiment

Prior to sealing the glove box, its interior walls, the surface of the entire chamber, theQMS and the glove box window have been all wiped and cleaned with isopropyl.

The working area inside the chamber has been prepared by placing the tools neededfor cleaving and fixing the olivine samples (i.e. tweezers, carbon tape, scissors, a smallvice, screwdrivers, a wrench, paper, the sample holders, a small fan and two nodules ofperidotite that contain the olivine crystals).

Further on, the glove box was sealed down, the gloves installed, leaving the systemready to be purged (see section 3.2.3 Purging the glove box).

4.1.1 Handling the olivine samples

The reason why the rocks containing the olivine crystals were broken apart inside theinert atmosphere of the glove box was to avoid the freshly cloven surfaces to react withthe atmospheric oxygen or to attract atmospheric moisture.

The method used to prepare the samples was used by Jonas Olsson back in 2009 andby Asmus Koefoed in 2011; a small sheet of paper was folded, forming a cup shape and apiece of peridotite was placed into one of the paper’s folds. In this way, the rock held bythe paper was fixed onto the vice (Fig. 4.1) and force was applied until it broke into tinypieces.

Peridotite is made up of forsterite (Mg2SiO4) - light green crystals, aluminium diopside(Ca(Mg,Fe,Al)(Si,Al)2O6) - dark green crystals and enstatite (Mg2Si2O6) - the brown-greenish ones, as identified and described by Jonas O. [31]. Using tweezers only smallforsterite crystals, of sizes between 1 and 3 mm, were selected, aiming towards selecting

Preliminary results 67

exclusively those who previously were located in the rock interior and not somewhere atits surface, which has been exposed to the laboratory conditions for years.

Fig. 4.1: Cleaving the olivine with the vice

Under mechanicalstress, olivine displays conchoidal fracture,i.e. it does not break along prominentcleavage directions, and this often resultsin a curved but smooth fracture surface [31].Therefore, a very close look over the selectedcrystals helped to determine which ones hada relatively flat surface and those were pickedup and mounted on the sample holder.

4.1.2 Mounting theolivine on the sample holder

Three sets of olivine samples have beenprepared during the experiment: the first twosample sets have been chosen to be insertedon the sample holder tray, one set beingpositioned under direct UV radiation andthe other set, under indirect UV radiationas reflected off of interior surfaces of thevacuum chamber. The third sample was keptinside the glove box but outside the vacuumchamber during the duration of the experiment. The crystals which were put inside thechamber were fixed on the tray using carbon tape as it is shown in Fig. 4.2.

Fig. 4.2: Olivine samples fixed with carbon tape to the sample holder; the set of samples to theright were put under direct UV irradiation while the left set of samples were exposed onlyindirectly to UV irradiation


4.2 Irradiation of the samples

Fig. 4.3: Front view (a) and side view (b) of the tilted sample holder

The samples were fixed on the sample holder, which has been tilted to approximately55o (Fig. 4.3a) in order to increase the area exposed to the ultraviolet flux. The Xe arclamp was positioned near the lateral viewport of the chamber, allowing a direct intenseillumination of the sample tray (Fig. 4.3b).

To receive the maximum flux of radiation, the samples were placed on the upper halfof the tray (viewed as it was tilted). As it is shown in Fig. 12.3.b, it is recommended toposition the samples above the orange line.

4.2.1 Limitations of the experiment

The main limitation during the conducted experiment was the potential overheatingof the chamber because of the continuous illumination of the very powerful Xe lamp.

This overheating allowed continuous irradiation sessions of only 3-4 hours, when thelamp had to be switched OFF for 1-2 hours to permit the cooling-down of the wholeset-up. The cooling system made of the stacked Peltier elements was not powered duringthese sessions, so that the only cooling of the sample holder was given by the cold watercirculating through the tubes installed beneath the sample holder.. Prior measurementson how much the cold water flow affects the temperature in the chamber were taken, anda cooling of aproximately 5oC was observed. The sample holder’s surface measured 17oC,


while the ambiental temperature was 22oC. Therefore, the cooling induced by only by thecirculating water was very low relative to the intense heating of the lamp.

Not having a functional humidity sensor which would have been very helpful, byindicating variations of the relative humidity inside the chamber, the pressure transducerwas the only device indicating real-time thermodynamic changes, in this case pressureincreases.

The maximum temperature supported by the transducer is 85oC, so any temperaturehigher than had to be avoided by all means.

By using the ideal gas law

pV = nRT (4.1)

for the initial state of the set-up

piV = Ti (4.2)

(where pi was the pressure in the chamber before the lamp was turned ON and Ti wasconsidered to be equal with the room temperature, measured to be 22.5oC (=295.64K) )and for the final state of the set-up (where T_max = 85oC ( = 358K))

pmaxV = Tmax (4.3)

it was easy to determine the value of pmax when the lamp had to be turned OFF.

pmax = Tmax/V (4.4)

The irradiation of the samples lasted 6.5 days, with the lamp being started for anaverage of 7 hours/day. There were 38 hours of irradiation in total.

4.3 Sample analysis

Fig. 4.4: Olivine samples coated with gold

During the 7th day of experiment,the pressure inside the chamber startedto increase rapidly (ca.1mbar/sec) sothat the experiment session had to beinterrupted and the samples were takenout. The cause of this major leak is notknown at the moment of the writing butit is believed that the VITON O-ringsituated close to the Xe lamp may havebeen affected.

The samples were removed from thesample holder and introduced in smallplastic sealed containers (resemblingsmall plastic bottles) and kept thereuntil they were coated with gold, and


later, analyzed by the SEM.

Coating the samples with goldOlivine is a very poor electric conductor, so in order to be analyzed with the scanning

electron microscope it has to be coated with aconducting mterial. We used gold becauseit is highly conductive and a thin layer of 50nm is enough to allow an efficient scanningof the microscope without any excess charge build-up. The coating session as well as theSEM operation were conducted by Jonas Olsson, with the author closely assisting him.

The purpose of the Olivine Experiment was to observe if any secondary products candevelop on freshly cleaved olivine crystals kept under an enriched CO2 atmosphere andirradiated by high intensity ultraviolet radiation. In this section, the results of SEManalysis are presented by presenting the three sample sets, evaluating them independentlyand enhancing the behaviour of the directly irradiated samples in contrast to the othertwo sets of samples. The results are shown as two images per page, starting with thedirectly irradiated samples, followed by the indirectly irradiated and those not exposed toUV, but present as witness samples in the glove box environmental conditions.

Selected images obtained during the SEM analysis are presented in this section in thefollowing order:

Fig. 4.5 Directly irradiated crystals:4.5.1a. Full view of the crystal 1 where lighter stains can be observed on the surface4.5.1b. Zoomed in boundary area between two different facades of the crystal showing afinely-grained covered area against the surrounding clean areas

4.6.2a. Full view of the crystal 2. The encircled area is zoomed in below4.6.2b. Zoomed area of the convergence of three faces of the crystal. An old face of thecrystal can be recognized in the bottom of the image where the sponge-like structureindicates cavities formed by the stress formed by trapped gas bubbles inside the crystalstructure [this statement results from a discussion with Jonas Olsson regardingphysically and chemically altered olivine surfaces]. The other two clean faces have beenrecently cloven.

4.7.4. and 4.7.5. Zoomed in areas of the directly irradiated crystals 4 and 5, showing lowdensities of granular structures.

4.8.1a. and 4.8.1b. Two different resolution images of the indirectly irradiated crystal 1.In Fig. 4.8.1a remnant crumbles resulting from the cracked pieces can be seen.

Fig.4.8.1b presence of a structure different than the granular type; it can be another typeof secondary product or it can be also induced by the coating.

Fig. 4.9.2a, 2b, 2c and 2d show the surface of the same directly illuminated crystal, butwhich was facing away so it was under indirect radiation only. The images are atdifferent resolution levels and they all display an enhancement of what appears as adensely packed granular layer, which has developed on the surface.

Fig. 4.10.3 depicts a patch of ordered grains on the surface of crystal 3 (indirect flux).The dark rectangle is an alteration of the surface produced by the highly focused beamof electrons emitted by the SEM, i.e. this is just an artefact of intense observation in the


SEM.Fig. 4.10.5 represent a zoomed in area from the surface of crystal 5, where a similargranular layer is present as well. The straight trench-like structures seen in the right halfof the image are intrinsic fracture lines of the crystal already present before irradiation.

Fig. 4.11.1a and 1b represent spherical grains disposed randomly on the surface of oneof the crystals kept in the glovebox environment. These grains are the ones that mostlyresemble the grains observed by Asmus Koefoed on the surface of his samples kept out ofdirect irradiation. Their nature cannot be stated as they have not yet been identified, butit seems that quite possibly these grains represent the first stage of secondary productsformation.Fig. 4.12.2a and 2b show highly ordered grain texture patterns at different resolutionsdeveloped on the surface of the glove box crystal 2, which was in the glove box duringthe experiment.

Because the crystals haven’t been cleaned after the peridotite nodule was broken, all ofthem contain small pieces ’contaminant’ consisting of remnant olivine ‘crumbles’ resultedfrom the fracturing of the mineral crystals but they are relatively easily distinguishable andcertainly in no way resemble the grains producing the texture patterns described above.They do therefore not pose a problem for interpretation.

During the analysis process, at least two distinctive structures could be observed. Forthe granular-structured layers, the diameter of the grains was measured to be between30nm and 230nm and they appeared being distributed randomly, without following acertain pattern. The other type of products found looked more as a conglomerate rice-likelayer, containing more elongated grains, larger than the previous type. Their length wasmeasured to be between 100nm and 660nm. However, in certain areas these elongatedgrains appeared not so dense and are not organized in highly ordered patterns.

Asmus Koefoed in 2011 [32] observed samples irradiated under similar conditions [32],and he found that the samples that were not under direct UV flux did developed similargrains types of grains on the surfaces as those found on the samples studied in the currentstudy; this can sustain the idea that the first more-likely to appear are microorganisms,which normally can show up on almost any type of surface if they meet suitable conditions.One interpretation is that microorganism can develop before any other possible chemicalreaction happens.

For the currently studied samples, the sizes and shapes of the new grains appearingon the surfaces, seemsto depend on whether these samples were kept under direct UVirradiation or out of the flux array, in the sense that the directly irradiated surfaces showa reduced density of these structures, while the other sets of samples show more intensifiedpopulations of newly formed grains.

The general idea formed after observing the samples, is that at least one type ofsecondary product showed up on the surface of the observed olivine crystals. The goldcoating might have influenced the samples’ surfaces to a certain level; but from e.g. Fig.12.5.1b where adjacent surfaces that were coated exactly in the same manner appearedto have completely different surface structure, it is obvious that, subsequently, also newstructures have developed.

The fact that the samples weren’t under continuous ultraviolet radiation is believed tobe the main reason that limited the secondary product formation to a premature stage ofdevelopment.


Fig. 4.5: 1a. Full image of the directly irradiated crystal 1; 1b. Zoomed in area of crystal 1


Fig. 4.6: 2a. Full image of the directly irradiated crystal 2; 2b. Zoomed in encircled area fromFig.2a


Fig. 4.7: 4. Zoomed in area of the directly irradiated crystal 4; 5. Zoomed in area of the directlyirradiated crystal 5


Fig. 4.8: 1a. Crystal 1 that was under indiirect UV radiation; 1b. Zoomed in area of the indirectlyirradiated crystal 1


Fig. 4.9: 2a. Crystal 2 that was under indiirect UV radiation; 2b, 2c, 2d. Zoomed in areas of theindirectly irradiated crystal 2


Fig. 4.10: 3.. Zoomed in area of the indirectly irradiated crystal 3; 5. Zoomed in areas of theindirectly irradiated crystal 5


Fig. 4.11: 1a., 1b. Zoomed in areas of the crystal 1 that was kept inside the GB


Fig. 4.12: 2a. Zoomed in area of the crystal 3 that was kept inside the GB; 2b. Zoomed in areasof the crystal 1 that was kept inside the GB

5Conclusion and recommendations

5.1 Conclusion

The task of building up a functional experimental set-up has been accomplished inthe sense that the present configuration of the NEW_JMMC can sustain Martianenvironmental simulations with relatively high accuracy.

After the construction of the chamber ended, an experiment aiming to investigate howfreshly cloven olivine surfaces react under CO2 atmosphere and very intense ultravioletradiation was conducted, and implicitly this experiment did confirm the capacity of theNEW_JMMC to sustain a controlled, Mars-like, environment.

However, the olivine experiment also revealed weak points of the set-up that canrelatively simply be overcome in the future. One of the insufficiencies was that twohumidity sensors failed to work properly. The consequence of this was that withouthaving a real-time transmission of the relative humidity, the cooling system was notstarted during the experiment. This triggered the temperature in the chamber toincrease due to the high intensity Xe arc lamp which didn’t allow continuous irradiationof the samples but cycles of 3-4 hours interrupted by 1-2 hours of cooling down pauseswhen the lamp was turned OFF. .

Regarding the assembly of the new chamber, it started with equipment parts used forthe 2011 prototype chamber, immediately after receiving the glove box from theChemistry Department. Having at our disposal a large versatile glovebox and a highquality quadrupole mass spectrometer (QMS) at the start of this project, has allowed thedevelopment of a more complex set-up than that of the 2011 JMMC. Throughout thebuilding process new ideas appeared and most of them ended-up being implemented inthe new installation. Among these are the cooling system for samples in thevacuum-chamber, the direct line of pure CO2 to the chamber and ”cracking” the controlof the glove-box, establishing all both electrical- and vacuum-feed-throughs to thechamber.

The next section presents a few aspects of this work that should be corrected and/orimproved in the future.

Conclusion and recommendations 83

5.2 Recommendations

The NEW_JMMC can still support many corrections and improvements. Once theOlivine Experiment has been conducted, the weak points showed up and somehow affectedthe ongoing experiment.

• The lack of a humidity sensor running correctly didn’t permit the use of the coolingsystem as it was desired. Once such a sensor will be installed in the chamber,transmitting real values of the humidity, it will be easier and safer to connect thePeltier elements that can bring an additional temperature drop of 20 oC. Currently,the only cooling inside the chamber has been given by the cold water running throughthe copper pipes, which usually have the role of a heat sink for the elements.

• By replacing the strong Xe arc lamp with a smaller and less powerful ultravioletsource would bring more than one advantage. For instance, by installing a UVLEDs array which emits UV light in the Martian range, on a small cooling system,the overheating of the chamber would be easily eliminated; being placed inside thechamber, the intense ozone creation would be strongly diminished. What is the mostimportant feature of this array is that it irradiates almost exactly in the Martianspectrum, so that should certainly be an add-on to the set-up.

• The water feed through at the chamber has to be shortened by a few centimeters (orbended to 90o) in order to have a good fitting of the set-up inside the glove box andto be able to mount the manually actuated VAT valve when the glove box windowis closed. Currently, the valve can be mounted when the window is there but then,it is impossible to get the sample holder out of the chamber.

• The olivine experiment was stopped because massive leaks were going on, mostprobably at one of the VITON O-rings, but the fact that the GB was flushed withnitrogen and argon beforehand, compensated this malfunction. Ar and N2 werethe gases infiltrating into the chamber and somehow not altering the quality of thevacuum to a great extent. A leak detection must be performed again and afterspotting the major leaking areas, damaged parts of the chamber can be replaced bybuying new ones.

• It would be a good idea to have the chamber equipped with an infrared thermocouplethat can detect local temperatures without making contact with any surfaces.

• The glove box operating system is still scarcely known and by understanding itbetter, this could offer many more advantages and facilitate processes like flushingthe glove box or control the moisture and oxygen levels inside it. Reinstalling thesoftware for the COROP OP15 electronic panel is also recommended.

• When a new olivine experiment is to be repeated, the samples should be intensivelycleaned with a strong jet of nitrogen in order to remove tiny crystal pieces that tendto stick to the faces of the sample. This suggestion came from Jonas Olsson who hasa long experience in studying the weathering of olivine.

LIST OF FIGURES

[1.1] The Windtunnel AWTS II, MarsLab, Åarhus, Denmark[1.2] Surface of Mars captured by Mastcam Right onboard of NASA’s Mars Rover

Curiosity on sol 107[1.3] First X-Ray view of Martian soil[1.4] Different types of olivine and their sources as exposed at the Geological Museum,

Copenhagen[2.1] Mass spectrum of the Martian atmosphere from sol 45[2.2] Gas composition spectrum after the injection of CO2 into the chamber[2.3] The PrismaPlus QMS attached to the NEW_JMMC[2.4] The operation principle of a QMF[2.5] Stability diagram of a QMF[2.6] Faraday stair spectrum of air taken with the PrismaPlus QMS inside the

NEW_JMMC[2.7] Faraday analog spectrum of air taken with the PrismaPlus QMS inside the

NEW_JMMC[2.8] PrismaPlus QMS’s analyzer[2.9] Field-axis technology[2.10] Faraday ion detector and SEM ion detector with discrete dynodes[2.11] Ok state of the Mass scale calibration[2.12] Coarse tuning of the Mass scale[2.13] Ion source tuning[2.14] Graphic representation of the electromagnetic spectrum[2.15] The extraterrestrial solar spectrum[2.16][2.17] Typical spectrum of the Martian disk[6.5] UV spectrum given by the Xe-lamp used as UV source at the NEW_JMMC[6.6][7.1][7.2][3.1] Moving of the glove box to the lab[3.2] Structure of alumino-silicates formed by corner-sharing of SiO4 and AlO4

tetrahedra[3.3] The oxygen and moisture probes[3.4] Pressure drop inside the antechamber[3.5] 8-way cross, clamps and flanges used at the NEW_JMMC[3.6] Main chamber-oven system (used to calculate the volume of the main chamber[3.7] Architecture of the back pump[3.8] Back pump pressure drop[3.9] Turbomolecular pump pressure drop[3.10] Sample holder in upright position and tilted position

[3.11] Set-up of the NEW_JMMC[3.12] Ping pong ball flow meter[3.13] Warning symbols for hazards likely to occur in the lab[3.14] Condensation on the surface of the TMP[3.15] Picture of the Xe arc lamp[4.1] Cleaving the olivine with the vice[4.2] Olivine samples fixed with carbon tape on the sample holder[4.3] Front and side views of the sample holder[4.4] Olivine samples coated with gold[4.5] Full image of the directly irradiated crystal and zoomed in area of crystal 1[4.6] Full image of the directly irradiated crystal 2 and zoomed in encircled area from

2a[4.7] Zoomed in area of the directly irradiated crystal 4 and zoomed in area of the

directly irradiated crystal 5[4.8] Crystal 1 that was under indiirect UV radiation and zoomed in area of the

indirectly irradiated crystal 1[4.9], [4.10] Crystal 2 that was under indiirect UV radiation and zoomed in areas of

the indirectly irradiated crystal 2[4.11] Zoomed in area of the indirectly irradiated crystal 3 and zoomed in areas of the

indirectly irradiated crystal 5[4.12] Zoomed in areas of the crystal 1 that was kept inside the GB[4.13] Zoomed in area of the crystal 3 that was kept inside the GB and zoomed in areas

of the crystal 1 that was kept inside the GB[9.2] Sketch of the glove box and antechamber and their metric dimensions[9.3] Photo of the UHV and the analyzer chambers[9.4] Representation of forces acting on the surface of the VAT valve’s gate

TABLES OF ABREVIATIONS AND NOTATIONS

ABREVIATIONSAFM = Atomic Force MicroscopyAU = Astronomical unitamu = atomic mass unitASTM = American Society for Testing and MaterialsDC = Direct CurrentGB = Glove BoxHEPA = High Efficiency Particulate AirISO = International Organization for StandardizationJMMC = Jens Martin Mars ChamberMAA = Martian Analog AtmosphereMSL = Mars Science LaboratoryNEW_JMMC = the new version of the Jens Martin Mars ChamberOIS = Open Ion Sourceppm = parts per millionQMA = Quadrupole Mass AnalyzerQME = Quadrupole Mass ElectronicsQMF = Quadrupole Mass FilterQMS = Quadrupole Mass SpectrometerRF = Radio FrequencyRGA = Residual Gas AnalysisSEM = Secondary Electron Multiplier (when mentioned under the

Quadrupole Mass Spectrometry chapter)Scanning Electron Microscope (when mentioned under theThe Olivine Experiment chapter)

SNC = group of meteorites: Shergottites, Nakhlites and ChassignitesTMP = Turbomolecular PumpTLS = Tunable Laser Spectrometer

NOTATIONSA= Ampere, unit of electric currentC = Coulomb, unit of electrical chargeFν= radiation fluxr0 = quadrupole field radiushν = energy of a photonν = wave frequencyh = Planck’s constant (= 6.626 x 10−34 J · s)

Bibliography

[1] QUADERA HTML Help Program Version 4.00. Quadera, 2009.

[2] Silas Boye Nissen. Is the color of Mars due to UV radiation? Master Thesis, 2012.

[3] Created by the Department of Geology at the University of Minnesota. Olivine group- Orthosilicate, 2012.

[4] Barth C.A. The Atmosphere of Mars. Annual Review of Earth and Planetary Sciences,2: 333-367, 1974.

[5] A. Chilingarov. Operation of two stacked Peltier elements.

[6] Peter H. Dawson. Quadrupole Mass Spectrometry and its applications. Amsterdam-Oxford-New York: Elsevier Scientific Publishing Company, 1976.

[7] Miller Philip E. and Denton M. Bonner. The Quadrupole Mass Filter: Basic operatingconcepts.

[8] Baptista Goncalo et al. Experimental study on oxygen and water removal fromgaseous streams for future gas systems in LHC detectors.

[9] Bish D.L. et al. X-ray diffraction results from Mars Science Laboratory:Mineralogyof Rocknest at Gale Crater. Science, 341, 2013.

[10] Blake D.F. et al. Curiosity at Gale Crater, Mars: Characterization and analysis ofthe Rocknest Sand Shadow. Science, 341, 2013.

[11] C.A. Barth et al. Mariner 6 and 7 Ultraviolet Spectrometer Experiment: Upperatmosphere data. Journal of Geophysical Research, 76, 2012.

[12] Ecrenaz T. et al. Hydrogen peroxide on Mars: Observations, interpretation and futureplans. Planetary and Space Science, 68:3–17, 2012.

[13] Elliott H.M. et al. The Michigan Mars Environmental Chamber: determining theconditions at which liquid brines form on Mars. 43rd Lunar and Planetary ScienceConference, 2012.

[14] Jensen LL. et al. A facility for long-term Mars simulation experiments: the MarsEnvironmental Simulation Chamber (MESCH). Astrobiology, 8, 2008.

[15] Leshin L.A. et al. Volatile, isotope, and organic analysis of Martian fines with theMars Curiosity Rover. Science, 341, 2013.

[16] Mahaffy Paul R. et al. Abundance and isotopic composition of gases in the Martianatmosphere from the Curiosity Rover. Science, 341:263–266, 2013.

[17] Meslin P.-Y. et al. Soil diversity and hydration as observed by ChemCam at GaleCrater. Science, 341, 2013.

[18] Möller L.E. et al. Mars Environmental Chamber for dynamic dust deposition andstatics analysis. Lunar aThend Planetary Science XXXV, 2004.

[19] Morris et al. Mossbauer mineralogy of rock, soil, and dust at Gusev crater, Mars.Journal of geophysical research, 111, 2006.

[20] Nilton O. Renno et al. Possible physical and thermodynamical evidence for liquidwater at the Phoenix landing site. Journal of Geophysical Research, 114, 2009.

[21] Olsson J. et al. Olivine reactivity with co_2 and h2o on a microscale: Implicationsfor carbon sequestration. Geochimica et Cosmochimica Acta, 77:86–97.

[22] Patel M.R. et al. Ultraviolet radiation on the surface of Mars and the Beagle 2 UVsensor. Nature, 436, 2005.

[23] Smith P.H. et al. H2o at the Phoenix landing site. Science, 325:58–61.

[24] Sobolev Alexander V. et al. An olivine-free mantle source of Hawaiian shield basalts.Nature, 434:590–597.

[25] Yamamoto S. et al. Possible mantle origin of olivine around lunar impact basinsdetected by SELENE, journal = Nature geoscience, volume = 3, pages = 533-536year = 2010.

[26] Yen A.S. et al. Evidence that the reactivity of the martian soil is due to superoxideions. Science, 289, 2000.

[27] Brucker G. and Antwerp Van K. Comparison of Ion trap mass spectrometer andQuadrupole mass spectrometer. Granville-Phillips, Gas Analysis Products, 2009.

[28] Pfeiffer Vacuum GmbH. Know how/quadrupole mass filter.

[29] Pfeiffer Vacuum GmbH. Know how/Ion sources, 2014.

[30] DataQ Instruments. A guide to signal configuration, 2014.

[31] Olsson Jonas. Characterization of secondary mineral formation on olivine by surfacesensitive technics. Master Thesis, 2009.

[32] Asmus Koefoed. JMMC - Design, Development, Calibration and Preliminary Results.Master Thesis, 2011.

[33] Keppler H. Kohlstedt DL. and Rubie DC. Solubility of water in the alpha, beta andgamma phases of (Mg,Fe)(2)SiO4. Web of Science, 1996.

[34] National Renewable Energy Laboratory. Solar spectra: Standard air mass zero.

[35] National Renewable Energy Laboratory. Wehrli 1985 AM0 Spectrum.

[36] Martel L.M.V. Pretty Green Mineral – Pretty Dry Mars?, 2013.

[37] Biscuit Software Ltd. The Rock collector, 2004.

[38] SGE Analytical Science Pty Ltd. How electron multipliers work, 2013.

[39] Raymond E. March and John F.J. Toss. Quadrupole Ion Trap Mass Spectrometry -2nd Edition. Hoboken, New Jersey: John Wiley & Sons, Inc., 2005.

[40] mBraun. Standard glovebox - operating instructions.

[41] mBraun. Standard glovebox - operating instructions.

[42] mBraun. Inertgas technology - MB-MO-SE1 Moisture analyzer, 2012.

[43] mBraun. Inertgas technology - MB OX-SE1 Oxygen Analyzer, 2012.

[44] NASA/JPL-Caltech/Ames. First x-ray view of Martian soil, 2012.

[45] Journal of Physics D: Applied Physics. Quadrupole mass spectrometry of reactiveplasmas, 2014.

[46] The Open University. Small mars chamber, 2014.

[47] Service Instructions Pfeiffer Vacuum. Rotary vane pumps - uno/duo 016.

[48] Pfeiffer Vacuum. PrismaPlus. Compact mass spectrometer system qmg 220, 2007.

[49] Stanford Research Systems. Application note #9.

[50] NASA Technical Reports Server. Chamber for simulating Martian and terrestrialenvironments, 2009.

[51] Oyama Bonnie Vance I. and J. Berdah. The Viking gas exchange experiment resultsfrom Chryse and Utopia surface samples. Journal of Geophysical Research, 28:4669–4676, 1977.

[52] Hirschmann M.M. Withers A.C. and Tenner T.J. The effect of Fe on olivine h2ostorage capacity: Consequences for h2o in the Martian mantle. American Mineralogist,96:1039–1053.

6Appendices

6.1 Appendix A

It is not a necessity to exactly determine the volumes of different parts from whichthe NEW_JMMC is built up at the present stage of measurements and experiments thatare conducted. However, knowing these volumes might become a must in the future whenfurther measurements will be conducted or when the pressure transducer has to be usedfor other tasks, so that knowing the volumes of e.g. the UHV or main chamber will beimportant.

Approximate determinations of the main chamber, UHV and analyzer chambervolumes have been done, the lack of higher precision being due to the fact that hoses,solenoid valves and irregular form cavities couldn’t be removed during the measurements.

Volumes of the glove box and antechamber

Fig. 6.1: Sketch of the glove box and antechamber indicating their metric dimensions

The volume of the glove box while being empty (recirculation fan and filter trap arestill included) has been calculated, considering the measurements shown in the Fig. 9.2,to be approximately 795 l.

The volume of the antechamber, which is a cylinder having a length of 60 cm and adiameter of 39 cm, is approximately 71 l.

Volumes of the UHV and analyzer chambers

The volumes of the UHV chamber and of the analyzer chamber have been deduced bysimply measuring the radius and the height of the adapting pieces and computing themas added cylindrical volumes.

Volume of the UHV chamber: VUHV=v1+v2 => VUHV=0.644 lVolume of the analyzer chamber Vanalyzer=v1+v2+v3+v4+v5 => Vanalyzer=1.05l

Fig. 6.2: Photos of the UHV chamber (1.) and of the analyzer chamber (2.)

Finding the forces acting on the two VAT valves’ gates

I. Finding the force acting on the gate of the manually actuated VAT valve

Considering the normal atmospheric pressure (P=101325 Pa) acting on the surface ofthe gate of the VAT valve (A=0.007m2) and the pressure p inside the main chamber atfull vacuum being p=-25 Pa, it was found that the force pressing on the gate is F=709.45N, which equals to 72.34 kg.

II. Finding the force acting on the automatic VAT valve when there is a pressuredifference ∆p between the UHV chamber and the main reaction chamber

Such situations can happen when a pressure difference exists between the UHV chamberand the main reaction chamber; under any circumstances, the VAT valve should not beopened if this pressure is larger than 10mbar as the TMP could be seriously damaged. Athigh pressure differences, the VAT itself would not operate correctly (e.g. will not opencompletely) and after a few attempts it can be damaged as well.

However, for as long as it remains closed, different pressures can exist in the twoseparated volumes and the force pressing from the higher pressure-side can be found usingthe following relation:

F = ∆p · area (6.1)

(the area of the gate of the VAT valve is 0.007 m2)

Fig. 6.3: Representation of forces acting on the surface of the VAT valve’s gate (1.) and photo ofthe automatic VAT valve (2.)

Detecting the order of the pins at the electrical feedthrough

Fig. 6.4: Sketch of the pin’s distribution

A 12 wire ribbon-cable has been used tomake the electrical connection between thechamber and the wires of the Peltier elementsand those of the Arduino board, which are allsituated outside the glove box.

The ribbon cable has been connectedto the multi-pin feedthrough which has acircular-locking connector on the air-side anda circular connector on the vacuum-side. Thefeedthrough has 16 pins in total, each of themhaving a number associated (i.e. from 1 to16) which have to be found in order to obtaina correct wiring.

The pins can very easily be detected usinga digital multimeter. As it is shown in the Fig.6.4, the numbering starts in the center of the connector and follows a circular path alongthe next two levels. The red dot on the connector stands as a reference point for the user.The wires of the ribbon cable have been coupled two-by-two in order to obtain six largerwires, thus increasing their resistance.

6.2 Appendix B

Operating procedures during the Olivine Experiment

This section gradually describes the maneuvers done during the olivine experiment.The emphasis is put on the spectra taken while the MAA was created.

Unlike during the preliminary tests of vacuum creation when normal atmosphericconditions surrounded the chamber, this time the presence of the inert atmosphere in theglove box made up mostly of Ar, with probably significant concentrations of N2 wassensed by the QMS. The infiltration of these gases was due to the leaks occurring aroundthe chamber.

This can be clearly seen in Fig. 6.1a and Fig.6.1b, which show ion current detectionsfor Ar around 0.1000 [E-07 A] after 20min of pumping and around 0.1170 [E-07 A] after1h of pumping, respectively.

After 1h of running the BP and TMP, they were switched OFF and the VAT valve wasclosed. After the TMP spinned down, the Xe lamp was turned ON for 30 minutes. Forunknown reasons, the QMS gives erroneous measurements when the lamp is ON so thatthe filament of the QMA was OFF during this time.

After the 30 passed, counting for photodissociation and further evaporation of watermolecules induced by the lamp , new spectra was taken after the pump were put again infunction.

At the end of this stage, it was observed that the pressure in the chamber and thespectra peaks were hardly changing so the chamber was opened and the sample tray wastaken out. This time inert gases (from the GB) filled it instead of the usual humid airfrom the lab. The blind flange was immediately put back on until the olivine sampleswere prepared and fixed on the sample holder. Once the olivine was inserted into thechamber, the steps described above were repeated. When the vacuum reached a stabilevalue (Fig.6.3.), CO2 was let into the system up to a pressure of 21 mbar.

Fig. 6.5: Ar presence after 20 min of pumping

Fig. 6.6: Increased peak of Ar after 1h of pumping

Fig. 6.7: Gas composition after the olivine was put inside the chamber, after 30 min. of pumping

By letting into the analyzing chamber a small amount of simulated MAA, a changein the CO2 concentration (Fig. 6.4) could be seen, although the pumps did very rapidlyejected this amount of gas.

Fig. 6.8: Variation of CO2 concentration

Fig. 6.8 shows a sudden drop in the ion current values at a specific time. However, thisis not a realistic decrease of the currents but a false feedback send by the analyzer at themoment when the small amount of CO2 was permitted to enter the analyzing chamber.It can be seen that in a few seconds, which is the reaction time of the QMA, the realpercentages were indicated again with only the CO2 level being higher than before.

6.3 Appendix C

In this section are shown further images obtained during the SEM session.

Fig. 6.9: 1a, 1b, 1c, 1d - Crystal surfaces exposed to direct UV radiation

Fig. 6.10: 1a, 1b - Crystal surfaces exposed to indirect UV radiation

Fig. 6.11: 1a, 1b - Crystal surfaces exposed the glovebox environment

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U High Accuracy ±0.08% BSL Includes Linearity, Hysteresis, and RepeatabilityU Broad Temperature Compensated Range -29 to 85°C (-20 to 185°F)U Premium Temperature Performance Span: ±0.5% Over Compensated RangeU 5-Point NIST Traceable Calibration IncludedU All Stainless Steel Wetted PartsU Fast Response TimeU Solid State Reliability and StabilityU 400% Proof Pressure Minimum

OMEGA’s PX409 Series high accuracy uni-directional vacuum range (negative gage pressure) models have all stainless steel wetted parts and welded construction and premium temperature compensation which makes them suitable for use in tough industrial environments. Vacuum models measure negative gage pressure with increasing output for increasing negative pressure. Ranges are from -10 inH2O to -15 psi with uni-directional outputs of 10 mV/V, 0 to 5 Vdc and 4 to 20 mA (ambient set at 4 mA).

SPECIFICATIONSOutput: Millivolt: 0 to 10 mV/V for vacuum Amplified Voltage: 0 to 5 Vdc for vacuum Current Loop: 4 to 20 mAPower Requirements: Millivolt: 5 to 10 Vdc (2 mA @ 10 Vdc) Amplified Voltage: 10 to 30 Vdc @ 10 mA Current Loop: 9 to 30 Vdc [max loop res = [(Vs-9) x 50] [9 to 20 Vdc above 105°C (229°F)]CE Compliant: Meets industrial emission and immunity standard EN61326Accuracy (Combined Linearity, Hysteresis and Repeatability): ±0.08% BSL maxZero Balance: ±0.5% FS typical 1% max (1% typical, 2% max for ranges 1 psi and below)Span Setting: ±0.5% FS typical 1% max (1% typical, 2% max for ranges 1 psi and below) calibrated in vertical direction with fitting downOperating Temperature Range: -45 to 121°C (-49 to 250°F) [-45 to 115°C (-49 to 240°F) for voltage or current outputs]Compensated Temperature: Ranges >5 psi: -29 to 85°C (-20 to 185°F) Ranges ≤5 psi: -17 to 85°C (0 to 185°F)Thermal Effects Zero (@ 0 psig Over Compensated Range): Ranges >5 psi: ±0.5% span Ranges ≤5 psi: ±1.0% span

Thermal Effects Span (Over Compensated Range): Ranges >5 psi: ±0.5% span Ranges ≤5 psi: ±1.0% spanLong Term Stability (1-Year): ±0.1% FS typicalShock: 50 g, 11 mS half sine, vertical and horizontal axis Vibration: 5-2000-5 Hz, 30 minute cycle, Curve L, Mil-Spec 810 figure 514-2-2, vertical and horizontal axisResponse Time: <1 msBandwidth: DC to 1 kHz typicalProof Pressure (positive direction): 10 inH2O: 10 times full scale 1 psi: 6 times full scale 2.5 psi and Higher: 4 times full scale (Negative direction 4 times or 1 atmosphere whichever is greater)Burst Pressure: 10 inH2O to 5 psi: 1000 psi 15 and Higher: 3000 psiElectrical Termination: PX409: Integral 2 m (6') cable PX419: mini DIN PX429: Twist-lock PX459: M12 4-pinsMating Connectors: PX419: CX5302 (included) PX429: PT06F10-6S (sold separately)Environmental Protection: PX409: IP67 PX419, PX429 and PX459: IP65Wetted Parts: 316 SSPressure Port: 1⁄4-18 NPT maleCalibration: Comes with 5-point calibration certificateWeight: 115 to 200 g (4 to 7 oz) depending upon configuration

IP67 ratedPX409-015VV 0 to -15 psi vaccum range shown actual size.

IP65 ratedPX419-001V5V 0 to -1 psi vacuum range shown actual size.

mini DIN style.

Cable style.

Standard

PX409 Series

Metric threads available, see omega.com/pxconfig

B-19

HIGH ACCURACY TRANSDUCERSwITH VACUUm PRESSURE RANGES

Custom Models Available!U Use Our Convenient On-Line Transducer Configurator to Choose the Features You WantU Visit omega.com/pxconfig for Details

PX419-015VI

PX429-015VV

All models shown smaller than actual size.

PX409-005V5V

Product Label

Hex 22 (0.87) AF��18 NPT

Pressure Adaptor

22(0.88)

79 (3.1)

79 (3.1)

��18 NPTPressure Adaptor

Hex 2.5 (1.0) AF

Conduit back end PXM409C

Integral cable back end PXM409

28(1.1)

5(0.2)

Twist lock back end PXM459

Vent withporous plug

(gage units only)

mini DIN back end PXM419

5(0.2)

M1

2x1

Ø 2

0.2

0.8

5(0.2)

22(0.88)

Vent with porous plug(gage units only)

Glass to medal sealed pins PXM4495

(0.2)

Integral cable back end PXM409

9(0.354)

Dimensions: mm (inch)

Twist-lock style.

Comes complete with 5-point NIST traceable calibration, calibrated with electrical connection up.* To order cable version with 1⁄2 NPT conduit fitting, specify model PX409C, no extra cost. ** To order with 0 to 10 Vdc output change “5V” to “10V” in model number, no extra cost. Metric threads and ranges also available, visit omega.com/pxconfigOrdering Examples: PX409-015VV, cable termination, 0 to -15 psig vacuum range, 10 mV/V output.PX459-001V5V, M12 termination, 0 to -1 psi vacuum range, 0 to 5 Vdc output.

ACCESSORIES MODEL NO. DESCRIPTION M12C-PVC-4-S-F-5 PVC cable, straight 4-pin M12 female connector one end, flying leads one end, 5 m (16.4') long, for PX459 M12C-PVC-4-R-F-5 PVC cable, right angled 4-pin M12 female connector one end, flying leads one end, 5 m (16.4') long, for PX459

mini DIN style.

Cable style.

To Order Visit omega.com/px409_vac for Pricing and Details VACUUM (NEGATIVE GAGE) RANGES RANGE psi VACUUM mbar 2 m (6') CABLE mini DIN TWIST-LOCK M12 CONN. NEGATIVE GAGE GAGE TERMINATION TERMINATION TERMINATION TERMINATION PRESSURE PRESSURE MODEL NO.* MODEL NO. MODEL NO. MODEL NO. 0 to 100 mV (@ 10 Vdc) OUTPUT 0 to -10 inH2O 0 to -25 PX409-10WVV PX419-10WVV PX429-10WVV PX459-10WVV 0 to -1 0 to -69 PX409-001VV PX419-001VV PX429-001VV PX459-001VV 0 to -2.5 0 to -172 PX409-2.5VV PX419-2.5VV PX429-2.5VV PX459-2.5VV 0 to -5 0 to -345 PX409-005VV PX419-005VV PX429-005VV PX459-005VV 0 to -15 0 to -1034 PX409-015VV PX419-015VV PX429-015VV PX459-015VV 0 to 5 Vdc OUTPUT** 0 to -10 inH2O 0 to -25 PX409-10WV5V PX419-10WV5V PX429-10WV5V PX459-10WV5V 0 to -1 0 to -69 PX409-001V5V PX419-001V5V PX429-001V5V PX459-001V5V 0 to -2.5 0 to -172 PX409-2.5V5V PX419-2.5V5V PX429-2.5V5V PX459-2.5V5V 0 to -5 0 to -345 PX409-005V5V PX419-005V5V PX429-005V5V PX459-005V5V 0 to -15 0 to -1034 PX409-015V5V PX419-015V5V PX429-015V5V PX459-015V5V 4 to 20 mA OUTPUT 0 to -10 inH2O 0 to -25 PX409-10WVI PX419-10WVI PX429-10WVI PX459-10WVI 0 to -1 0 to -69 PX409-001VI PX419-001VI PX429-001VI PX459-001VI 0 to -2.5 0 to -172 PX409-2.5VI PX419-2.5VI PX429-2.5VI PX459-2.5VI 0 to -5 0 to -345 PX409-005VI PX419-005VI PX429-005VI PX459-005VI 0 to -15 0 to -1034 PX409-015VI PX419-015VI PX429-015VI PX459-015VI

Metric threads available, see omega.com/pxconfig

www.mbraun.com

STANDARD GLOVEBOX WORKSTATIONS

Programmable Logic Controller

Light Hood

Adjustable Shelving

Glove Ports

Castors for Easy Mobility

Leveling Feet

Large Antechamber

Flange DN 40 KF

*Small Antechamber

Stainless Steel Piping

Gas Purification System

Vacuum Pump

Foot Switch

*Freezer

*Freezer

Light Hood

Adjustable Shelving

*Analyzers

*Analyzers

Gas Purification System

Touch Screen PLC Controller

Stainless Steel Piping

*Small Antechamber

Large Antechamber


Leveling feet

Flange DN 40 KF

Fine Filter

Fine Filter

Foot Switch

Glove Ports

*LABstar glovebox workstation is pictured with optional features

*UNIlab glovebox workstation is pictured with optional features

Flow Meter

GLOVEBOX CONFIGURATIONS MAY VARY

MB

RA

UN

GLO

VE

BO

X W

OR

KS

TAT

ION

*LABmaster SP/DP glovebox workstation is pictured with optional features

Gas PurificationSingle (SP) or Double (DP) Purifier Unit

Color Touch Screen PLC Controller

*Small Antechamber

Large Antechamber

Leveling Feet

Flange DN 40 KF

Light Hood

Adjustable Shelving

Glove Ports


Foot Switch

Vacuum Pump

*External Solvent Trap

Fine Filter

LABstar Standard Features:• Programmable logic controller• Large main antechamber• Three glovebox sizes available• Vacuum pump• Automatic regenerable H2O/O2 single column inert gas purifier• World-wide operation using standard power supply• Integrated high vacuum feedthroughs• Stainless steel adjustable shelving• Stainless steel piping

LABstar Optional Features:• Mini-antechamber• H2O/O2 analyzer• Freezer• Box filter with activated charcoal• Microscope equipment• Dry scroll pump• Automatic antechamber controls• PLC controller with touch screen monitor• Auto purge function• Other options available

UNIlab Standard Features:• PLC controller with touch screen monitor• Large main antechamber• Three glovebox sizes available• Vacuum pump• Automatic regenerable H2O/O2 single column inert gas purifier• World-wide operation using standard power supply• Integrated high vacuum feedthroughs• Stainless steel adjustable shelving• Stainless steel piping

UNIlab Optional Features:• Mini-antechamber• H2O/O2 analyzer• Dry scroll pump• Freezer• Box filter with activated charcoal• External solvent absorber• Auto purge function• Microscope equipment• Automatic antechamber controls• Other options available

LABmaster SP/DP Standard Features:• A variety of modular glovebox sizes available• PLC controller with color touch screen monitor• Large main antechamber• Vacuum pump• Automatic regenerable H2O/O2 single (SP) / double (DP) column inert gas purifier• World-wide operation using standard power supply• Integrated high vacuum feedthroughs• Stainless steel adjustable shelving• Stainless steel piping

LABmaster SP/DP Optional Features:• Mini-antechamber• H2O/O2 analyzer• Freezer• Vacuum oven 250°C and 600°C• Box filter with activated carbon• External solvent absorber• Dry scroll pump• Microscope equipment• Mechanical door locks• Automatic antechamber controls• Auto purge function• Other options available

LABWORKSTATION

The LABstar workstation is a ready to operate high quality glovebox system that meets your specific application requirements. The LABstar workstation features a large main antechamber, 10 cfm vacuum pump, and programmable logic controller (PLC). Other standard features include an automatic regenerable oxygen and moisture single column inert gas purification system that purifies the glovebox atmosphere to levels of less than 1 ppm oxygen and moisture.

UNIWORKSTATION

The UNIlab workstation is the next step up from the LABstar workstation in the MBRAUN standard glovebox line. The UNIlab workstation is a ready to operate high quality glovebox that includes a large main antechamber, 10 cfm vacuum pump, and a PLC controller with touch screen monitor. The UNIlab workstation features an automatic regenerable oxygen and moisture single column inert gas purification system that purifies the glovebox atmosphere to levels of less than 1 ppm oxygen and moisture.

LAB SP/DPWORKSTATION

The LABmaster workstation offers additional features and benefits compared to the UNIlab and LABstar workstations. The LABmaster workstation is the top of the line glovebox featuring a modular workspace, large main antechamber, 10 cfm vacuum pump, and a PLC controller with color touch screen monitor.The LABmaster offers automatic regenerable oxygen and moisture gas purification systems with single or double filter columns that purify the glovebox atmosphere to levels of less than 1 ppm oxygen and moisture.

*LABstar glovebox workstation is pictured with optional features

*UNIlab glovebox workstation is pictured with optional features

*LABmaster SP/DP glovebox workstation is pictured with optional features

MBRAUN GLOVEBOX WORKSTATIONS

• Sizes (Internal Workspace)1200mm (L) x 780mm (D) x 920mm (H)1450mm (L) x 780mm (D) x 920mm (H)1950mm (L) x 780mm (D) x 920mm (H)

1200mm (L) x 780mm (D) x 920mm (H)1450mm (L) x 780mm (D) x 920mm (H)1950mm (L) x 780mm (D) x 920mm (H)

Lengths: 1250mm, 1500mm, 1800mm Depths: 780mm, 1000mm, 1200mm Height: 900mm Modular Sizes


• Modular in Design No No Yes Yes

• Material Stainless Steel 1.4301 (US Type 304) Stainless Steel 1.4301 (US Type 304) Stainless Steel 1.4301 (US Type 304) Stainless Steel 1.4301 (US Type 304)

• Feedthroughs (2) DN 40 KF Pieces Included (1) Electrical (2) DN 40 KF Pieces Included (1) Electrical (4) DN 40 KF Pieces Included (1) Electrical (4) DN 40 KF Pieces Included (1) Electrical

• Dust Filter (0.3 μm) (1) Gas Inlet, (1) Gas Outlet, Class H 13 (1) Gas Inlet, (1) Gas Outlet, Class H 13 (1) Gas Inlet, (1) Gas Outlet, Class H 13 (1) Gas Inlet, (1) Gas Outlet, Class H 13

• Windows Scratch Resistant Polycarbonate Scratch Resistant Polycarbonate Scratch Resistant Polycarbonate Scratch Resistant Polycarbonate

• Gloves (Optional Sizes Available) (1)Butyl .4mm Thick (1)Butyl .4mm Thick (1)Butyl .4mm Thick (1) Butyl .4mm Thick

• Glove Port (Oval Ports Available) POM 220mm Diameter POM 220mm Diameter POM 220mm Diameter POM 220mm Diameter

• Box Light Fluorescent Front Mounted Lamp Fluorescent Front Mounted Lamp Fluorescent Front Mounted Lamp Fluorescent Front Mounted Lamp

• Stainless Steel Shelving (3) 1000mm Length x 220mm Depth (3) 1000mm Length x 220mm Depth (2)(3) 1000mm Length x 220mm Depth (2)(3) 1000mm Length x 220mm Depth

• Leak Rate (Oxygen Method) <0.05 vol%h Typical (Class 1) <0.05 vol%h Typical (Class 1) <0.05 vol%h Typical (Class 1) <0.05 vol%h Typical (Class 1)

• Leak Rate (Press. Change Method) (3) <0.05 vol%h (Class 1) (3) <0.05 vol%h (Class 1) (3) <0.05 vol%h (Class 1) (3) <0.05 vol%h (Class 1)

• Type (4) Cylindrical w/ Stainless Steel Sliding Tray (4) Cylindrical w/ Stainless Steel Sliding Tray (4) Cylindrical w/ Stainless Steel Sliding Tray (4) Cylindrical w/ Stainless Steel Sliding Tray

• Size (Inside Dimensions) 390mm Diameter x 600mm Length 390mm Diameter x 600mm Length 390mm Diameter x 600mm Length 390mm Diameter x 600mm Length


• Door Aluminum Aluminum Aluminum Aluminum

• Vacuum (5) Manual Operation (5) Manual Operation (6)Push Button Evac. & Refill (6) Manual & Push Button Evac. & Refill Available

• Leak Rate <10-5 mbar l/s (Class 1) <10-5 mbar l/s (Class 1) <10-5 mbar l/s (Class 1) <10-5 mbar l/s (Class 1)

• Purifier Single Column Gas Purifier Unit Single Column Gas Purifier Unit Single Purifier (SP) / Double Purifier (DP) MB 20G, MB 200G, MB 300G & MB 600G available

• Attainable Purity H2O < 1 ppm, O2 < 1 ppm H2O < 1 ppm, O2 < 1 ppm H2O < 1 ppm, O2 < 1 ppm H2O < 1 ppm, O2 < 1 ppm

• Vacuum Pump (Dry Pump Available) 10 cfm Rotary Vane Pump 10 cfm Rotary Vane Pump 10 cfm Rotary Vane Pump 10 cfm Rotary Vane Pump

• Regeneration Auto Regeneration Auto Regeneration w/ Auto Restart Feature Auto Regeneration w/ Auto Restart Feature Auto Regeneration w/ Auto Restart Feature

• Capacity 20L O2 Removal &1000G H2O Removal

30L O2 Removal &1300G H2O Removal


30L up to 180L O2 Removal &1300G up to 3000G H2O Removal

• Main Valves Electro-pneumatic Electro-pneumatic Electro-pneumatic Electro-pneumatic

• Encapsulated Blower Single Speed without Frequency Controller Multiple Speeds with Frequency Controller Multiple Speeds with Frequency Controller Multiple Speeds with Frequency Controller

• Piping Stainless Steel 1.4301 (US Type 304) Stainless Steel 1.4301 (US Type 304) Stainless Steel 1.4301 (US Type 304) Stainless Steel 1.4301 (US Type 304)

• Flow Rate 20 m3/h at ∆P= 60 mbar 84 m3/h at ∆P= 60 mbar 84 m3/h at ∆P= 60 mbar 84 m3/h up to 310 m3/h at ∆P= 60 mbar

• Electrical Power 230 V/50-60 Hz, 10 A or 115 V /50-60 Hz, 20 A or 100 V/ 50-60 Hz, 20 A

230 V/50-60 Hz, 10 A or 115 V /50-60 Hz, 20 A or 100 V/ 50-60 Hz, 20 A



• Controller (7)Programmable Logic Controller PLC Control w/ Touch Screen Monitor PLC Control w/ Color Touch Screen Monitor PLC Control w/ Color Touch Screen Monitor

• Box Pressure Control Automatic Box Pressure Control w/ Foot Switch (+15 mbar, -15 mbar)Automatic Box Pressure Control w/ Foot Switch

(+15 mbar, -15 mbar)Automatic Box Pressure Control w/ Foot Switch


(+15 mbar, -15 mbar)

• Multi-language Operation Yes Yes Yes Yes

• Trending Capabilities Optional Feature Yes Yes Yes

• Touch Panel Design Optional Feature Yes Yes Yes

Glovebox

LargeAntechamber

Gas Purifier

LABstar Workstation

Controller

(1.) A variety of gloves (Hypalon, Neoprene and Butyl) and thickness sizes are available upon request. (2.) Double sided gloveboxes include 2 hanging shelves. Additional shelving options are available. (3.) < 0.05 vol%/h at negative pressure of 10 mbar at constant temperature (measured at final acceptance test) (4.) Square antechamber, L-chamber and T-chamber designs are available. (5.) Timed antechamber control can be included as an optional item. (6.) Timed antechamber control and fully automatic antechamber controls are available (7.) The Programmable Logic Controller can be upgraded to the optional touch screen interface.

MB

RA

UN

GLO

VE

BO

X D

IRE

CT

CO

MPA

RIS

ON

MBRAUN GLOVEBOX WORKSTATIONS

• Sizes (Internal Workspace)1200mm (L) x 780mm (D) x 920mm (H)1450mm (L) x 780mm (D) x 920mm (H)1950mm (L) x 780mm (D) x 920mm (H)

1200mm (L) x 780mm (D) x 920mm (H)1450mm (L) x 780mm (D) x 920mm (H)1950mm (L) x 780mm (D) x 920mm (H)



• Modular in Design No No Yes Yes


• Feedthroughs (2) DN 40 KF Pieces Included (1) Electrical (2) DN 40 KF Pieces Included (1) Electrical (4) DN 40 KF Pieces Included (1) Electrical (4) DN 40 KF Pieces Included (1) Electrical

• Dust Filter (0.3 μm) (1) Gas Inlet, (1) Gas Outlet, Class H 13 (1) Gas Inlet, (1) Gas Outlet, Class H 13 (1) Gas Inlet, (1) Gas Outlet, Class H 13 (1) Gas Inlet, (1) Gas Outlet, Class H 13

• Windows Scratch Resistant Polycarbonate Scratch Resistant Polycarbonate Scratch Resistant Polycarbonate Scratch Resistant Polycarbonate

• Gloves (Optional Sizes Available) (1)Butyl .4mm Thick (1)Butyl .4mm Thick (1)Butyl .4mm Thick (1) Butyl .4mm Thick

• Glove Port (Oval Ports Available) POM 220mm Diameter POM 220mm Diameter POM 220mm Diameter POM 220mm Diameter

• Box Light Fluorescent Front Mounted Lamp Fluorescent Front Mounted Lamp Fluorescent Front Mounted Lamp Fluorescent Front Mounted Lamp

• Stainless Steel Shelving (3) 1000mm Length x 220mm Depth (3) 1000mm Length x 220mm Depth (2)(3) 1000mm Length x 220mm Depth (2)(3) 1000mm Length x 220mm Depth

• Leak Rate (Oxygen Method) <0.05 vol%h Typical (Class 1) <0.05 vol%h Typical (Class 1) <0.05 vol%h Typical (Class 1) <0.05 vol%h Typical (Class 1)

• Leak Rate (Press. Change Method) (3) <0.05 vol%h (Class 1) (3) <0.05 vol%h (Class 1) (3) <0.05 vol%h (Class 1) (3) <0.05 vol%h (Class 1)

• Type (4) Cylindrical w/ Stainless Steel Sliding Tray (4) Cylindrical w/ Stainless Steel Sliding Tray (4) Cylindrical w/ Stainless Steel Sliding Tray (4) Cylindrical w/ Stainless Steel Sliding Tray

• Size (Inside Dimensions) 390mm Diameter x 600mm Length 390mm Diameter x 600mm Length 390mm Diameter x 600mm Length 390mm Diameter x 600mm Length


• Door Aluminum Aluminum Aluminum Aluminum

• Vacuum (5) Manual Operation (5) Manual Operation (6)Push Button Evac. & Refill (6) Manual & Push Button Evac. & Refill Available

• Leak Rate <10-5 mbar l/s (Class 1) <10-5 mbar l/s (Class 1) <10-5 mbar l/s (Class 1) <10-5 mbar l/s (Class 1)

• Purifier Single Column Gas Purifier Unit Single Column Gas Purifier Unit Single Purifier (SP) / Double Purifier (DP) MB 20G, MB 200G, MB 300G & MB 600G available

• Attainable Purity H2O < 1 ppm, O2 < 1 ppm H2O < 1 ppm, O2 < 1 ppm H2O < 1 ppm, O2 < 1 ppm H2O < 1 ppm, O2 < 1 ppm

• Vacuum Pump (Dry Pump Available) 10 cfm Rotary Vane Pump 10 cfm Rotary Vane Pump 10 cfm Rotary Vane Pump 10 cfm Rotary Vane Pump

• Regeneration Auto Regeneration Auto Regeneration w/ Auto Restart Feature Auto Regeneration w/ Auto Restart Feature Auto Regeneration w/ Auto Restart Feature

• Capacity 20L O2 Removal &1000G H2O Removal



30L up to 180L O2 Removal &1300G up to 3000G H2O Removal

• Main Valves Electro-pneumatic Electro-pneumatic Electro-pneumatic Electro-pneumatic

• Encapsulated Blower Single Speed without Frequency Controller Multiple Speeds with Frequency Controller Multiple Speeds with Frequency Controller Multiple Speeds with Frequency Controller

• Piping Stainless Steel 1.4301 (US Type 304) Stainless Steel 1.4301 (US Type 304) Stainless Steel 1.4301 (US Type 304) Stainless Steel 1.4301 (US Type 304)

• Flow Rate 20 m3/h at ∆P= 60 mbar 84 m3/h at ∆P= 60 mbar 84 m3/h at ∆P= 60 mbar 84 m3/h up to 310 m3/h at ∆P= 60 mbar

• Electrical Power 230 V/50-60 Hz, 10 A or 115 V /50-60 Hz, 20 A or 100 V/ 50-60 Hz, 20 A




• Controller (7)Programmable Logic Controller PLC Control w/ Touch Screen Monitor PLC Control w/ Color Touch Screen Monitor PLC Control w/ Color Touch Screen Monitor

• Box Pressure Control Automatic Box Pressure Control w/ Foot Switch (+15 mbar, -15 mbar)Automatic Box Pressure Control w/ Foot Switch



(+15 mbar, -15 mbar)

• Multi-language Operation Yes Yes Yes Yes

• Trending Capabilities Optional Feature Yes Yes Yes

• Touch Panel Design Optional Feature Yes Yes Yes

UNIlab Workstation LABmaster Workstation MOD Workstation

(1.) A variety of gloves (Hypalon, Neoprene and Butyl) and thickness sizes are available upon request. (2.) Double sided gloveboxes include 2 hanging shelves. Additional shelving options are available. (3.) < 0.05 vol%/h at negative pressure of 10 mbar at constant temperature (measured at final acceptance test) (4.) Square antechamber, L-chamber and T-chamber designs are available. (5.) Timed antechamber control can be included as an optional item. (6.) Timed antechamber control and fully automatic antechamber controls are available (7.) The Programmable Logic Controller can be upgraded to the optional touch screen interface.

UNIWORKSTATION

Weight = 400 kg / 600 kg

1950 mm (L) x 780 mm (D) x 920 mm (H)1200 mm (L) x 780 mm (D) x 920mm (H) 1450 mm (L) x 780 mm (D) x 920mm (H)

LAB SP/DPWORKSTATION


MOD-MODULAR WORKSTATION


LABWORKSTATION


1950 mm (L) x 780 mm (D) x 920 mm (H)1200 mm (L) x 780 mm (D) x 920 mm (H) 1450 mm (l) x 780 mm (D) x 920mm (H)

1250 mm (L) x 780 mm (D) x 900 mm (H) 1500 mm (L) x 780 mm (D) x 900 mm (H) 1800 mm (L) x 780 mm (D) x 900 mm (H)

1250 mm (L) x 780 mm (D) x 900 mm (H) 1500 mm (L) x 780 mm (D) x 900 mm (H) 1800 mm (L) x 780 mm (D) x 900 mm (H)

INT

ER

NA

L W

OR

KIN

G D

IME

NS

ION

S

Volume:

1250 (L) = 0.8 m3

1450 (L) = 1.0 m3

1950 (L) = 1.4 m3

Volume:

1250 (L) = 0.8 m3

1450 (L) = 1.0 m3

1950 (L) = 1.4 m3

EX

AM

PLE

S O

F GLO

VE

BO

X C

ON

FIGU

RA

TIO

NS

WIT

H G

AS

PU

RIFIE

RS

www.mbraun.com

Volume:

1250 (L) = 0.8 m3

1500 (L) = 1.0 m3

1800 (L) = 1.2 m3

Volume:

1250 (L) = 1.0 m3

1500 (L) = 1.2 m3

1800 (L) = 1.5 m3

Volume:

1250 (L) = 1.2 m3

1500 (L) = 1.5 m3

1800 (L) = 1.8 m3

Volume:

1250 (L) = 0.8 m3

1500 (L) = 1.0 m3

1800 (L) = 1.2 m3

Volume:

1250 (L) = 1.0 m3

1500 (L) = 1.2 m3

1800 (L) = 1.5 m3

Volume:

1250 (L) = 1.2 m3

1500 (L) = 1.5 m3

1800 (L) = 1.8 m3

Gas Purification System 300G

Gas Purification System 20G / 200G

Gas Purification System 20GGas Purification System 10G

EX

AM

PLE

S O

F GLO

VE

BO

X C

ON

FIGU

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M.Braun Inertgas-Systeme GmbH (Headquarters)Dieselstr. 31 • 85748 Garching • Germany

Phone: +49 89 32669-0 • Fax: +49 89 32669-105www.mbraun.de • [email protected]

Germany

M.Braun Incorporated 14 Marin Way • Stratham, NH • 03885

Phone: +1 603-773-9333 • Fax: +1 603-773-0008www.mbraunusa.com • [email protected]

USA

M.Braun West Coast OfficeSuite 206 • 2570 North First Street • San Jose, CA • 95131

Phone: +1 408-273-4594 • Fax: +1 408-273-4694www.mbraunusa.com • [email protected]

USA West Coast

M.Braun UK & IrelandMansfield Business Center • Ashfield Avenue • Mansfield

Nottinghampshire • NG18 2AE • United KingdomPhone: +44 1623 404329 • Fax: +44 1623 404277

www.mbraun.co.uk • [email protected]

UK & Ireland

M.Braun Inertgas Systeme Co. Ltd. (Shanghai)828 Xin Jinqiao Road • Pudong Shanghai 201206 • P.R.C

Phone: +86 21 5032 02 57 • Fax: +86 21 5032 02 29www.mbraunchina.com • [email protected]

China

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