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At least 19 records

Ultra Pure Water Cleaning Baseline Study on NASA JSC Astromaterial Curation Gloveboxes

Future sample return missions will require strict protocols and procedures for reducing inorganic and organic contamination in isolation containment systems. In 2012, a baseline study was orchestrated to establish the current state of organic cleanliness in gloveboxes used by NASA JSC astromaterials curation labs [1, 2]. As part of this in-depth organic study, the current curatorial technical support procedure (TSP) 23 was used for cleaning the gloveboxes with ultra pure water (UPW) [3-5]. Particle counts and identification were obtained that could be used as a benchmark for future mission designs that require glovebox decontamination. The UPW baseline study demonstrates that TSP 23 works well for gloveboxes that have been thoroughly degreased. However, TSP 23 could be augmented to provide even better glovebox decontamination. JSC 03243 could be used as a starting point for further investigating optimal cleaning techniques and procedures. DuPont Vertrel XF or other chemical substitutes to replace Freon- 113, mechanical scrubbing, and newer technology could be used to enhance glovebox cleanliness in addition to high purity UPW final rinsing. Future sample return missions will significantly benefit from further cleaning studies to reduce inorganic and organic contamination.

Calaway, Michael J.

Decontaminating Solar Wind Samples with the Genesis Ultra-Pure Water Megasonic Wafer Spin Cleaner

The Genesis sample return capsule, though broken during the landing impact, contained most of the shattered ultra-pure solar wind collectors comprised of silicon and other semiconductor wafers materials. Post-flight analysis revealed that all wafer fragments were littered with surface particle contamination from spacecraft debris as well as soil from the impact site. This particulate contamination interferes with some analyses of solar wind. In early 2005, the Genesis science team decided to investigate methods for removing the surface particle contamination prior to solar wind analysis.

Calaway, Michael J.

Cleaning Genesis Mission Payload for Flight with Ultra-Pure Water and Assembly in ISO Class 4 Environment

Genesis mission to capture and return to Earth solar wind samples had very stringent contamination control requirements in order to distinguish the solar atoms from terrestrial ones. Genesis mission goals were to measure solar composition for most of the periodic table, so great care was taken to avoid particulate contamination. Since the number 1 and 2 science goals were to determine the oxygen and nitrogen isotopic composition, organic contamination was minimized by tightly controlling offgassing. The total amount of solar material captured in two years is about 400 micrograms spread across one sq m. The contamination limit requirement for each of C, N, and O was <1015 atoms/sq cm. For carbon, this is equivalent to 10 ng/cm2. Extreme vigilance was used in pre-paring Genesis collectors and cleaning hardware for flight. Surface contamination on polished silicon wafers, measured in Genesis laboratory is approximately 10 ng/sq cm.

Allton, Judith H.

Rust Contamination from Water Leaks in the Cosmic Dust Lab and Lunar and Meteorite Thin Sections Labs at Johnson Space Center

On the early morning of September 15th, 2016, on the first floor of Building 31 at NASA-Johnson Space Center, the hose from a water chiller ruptured and began spraying water onto the floor. The water had been circulating though old metal pipes, and the leaked water contained rust-colored particulates. The water flooded much of the western wing of the building's ground floor before the leak was stopped, and it left behind a residue of rust across the floor, most notably in the Apollo and Meteorite Thin Section Labs and Sample Preparation Lab. No samples were damaged in the event, and the affected facilities are in the process of remediation. At the beginning of 2016, a separate leak occurred in the Cosmic Dust Lab, located in the same building. In that lab, a water leak occurred at the bottom of the sink used to clean the lab's tools and containers with ultra-pure water. Over years of use, the ultra-pure water eroded the metal sink piping and leaked water onto the inside of the lab's flow bench. This water also left behind a film of rusty material. The material was cleaned up and the metal piping was replaced with PVC pipe and sealed with Teflon plumber's tape. Samples of the rust detritus were collected from both incidents. These samples were imaged and analyzed to determine their chemical and mineralogical compositions. The purpose of these analyses is to document the nature of the detritus for future reference in the unlikely event that these materials occur as contaminants in the Cosmic Dust samples or Apollo or Meteorite thin sections.

Kent, J. J.

Continuous-Flow System Produces Medical-Grade Water

A continuous-flow system utilizes microwave heating to sterilize water and to thermally inactivate endotoxins produced in the sterilization process. The system is designed for use in converting potable water to medical-grade water. Systems like this one could be used for efficient, small-scale production of medical- grade water in laboratories, clinics, and hospitals. This system could be adapted to use in selective sterilization of connections in ultra-pure-water-producing equipment and other equipment into which intrusion by microorganisms cannot be tolerated. Lightweight, port - able systems based on the design of this system could be rapidly deployed to remote locations (e.g., military field hospitals) or in response to emergencies in which the normal infrastructure for providing medical-grade water is disrupted. Larger systems based on the design of this system could be useful for industrial production of medical-grade water. The basic microwave-heating principle of this system is the same as that of a microwave oven: An item to be heated, made of a lossy dielectric material (in this case, flowing water) is irradiated with microwaves in a multimode microwave cavity. The heating is rapid and efficient because it results from absorption of microwave power throughout the volume of the lossy dielectric material. In this system, a copper tube having a length of 49.5 cm and a diameter of 2.25 cm serves as both the microwave cavity and the sterilization chamber. Microwave power is fed via a coaxial cable to an antenna mounted inside the tube at mid-length (see figure). Efficient power transfer occurs due to the shift in wavelength associated with the high permittivity of water combined with the strong coupling of 2.45-GHz microwaves with rotational-vibrational transitions of the dipolar water molecule.

Akse, James R.

Microwave Sterilization and Depyrogenation System

A fully functional, microgravity-compatible microwave sterilization and depyrogenation system (MSDS) prototype was developed that is capable of producing medical-grade water (MGW) without expendable supplies, using NASA potable water that currently is available aboard the International Space Station (ISS) and will be available for Lunar and planetary missions in the future. The microwave- based, continuous MSDS efficiently couples microwaves to a single-phase, pressurized, flowing water stream that is rapidly heated above 150 C. Under these conditions, water is rapidly sterilized. Endotoxins, significant biological toxins that originate from the cell walls of gram-negative bacteria and which represent another defining MGW requirement, are also deactivated (i.e., depyrogenated) albeit more slowly, with such deactivation representing a more difficult challenge than sterilization. Several innovations culminated in the successful MSDS prototype design. The most significant is the antenna-directed microwave heating of a water stream flowing through a microwave sterilization chamber (MSC). Novel antenna designs were developed to increase microwave transmission efficiency. These improvements resulted in greater than 95-percent absorption of incident microwaves. In addition, incorporation of recuperative heat exchangers (RHxs) in the design reduced the microwave power required to heat a water stream flowing at 15 mL/min to 170 C to only 50 W. Further improvements in energy efficiency involved the employment of a second antenna to redirect reflected microwaves back into the MSC, eliminating the need for a water load and simplifying MSDS design. A quick connect (QC) is another innovation that can be sterilized and depyrogenated at temperature, and then cooled using a unique flow design, allowing collection of MGW at atmospheric pressure and 80 C. The final innovation was the use of in-line mixers incorporated in the flow path to disrupt laminar flow and increase contact time at a given flow rate. These technologies can be employed in small-scale systems for efficient production of MGW in the laboratory or in a range of larger systems that meet various industrial requirements. The microwave antennas can also be adapted to selectively sterilize vulnerable connections to ultra-pure water production facilities or biologically vulnerable systems where microorganisms may intrude.

Akse, James R.

Cleaning at the Edge of Science: NASA's Genesis Mission

As part of NASA's continuing exploration of the origins of our solar system, the California Institute of Technology, Jet Propulsion Laboratory, Lockheed Martin Astronautics, Los Alamos National Laboratory, and the Johnson Space Center are working together to develop the Genesis mission to return solar matter for analysis in terrestrial laboratories. These samples will be used to define a baseline for the chemical and isotopic composition of the solar nebula. Deviations from the baseline resulted as the solar system evolved; thus, providing a tracer for materials incorporated into meteorites, comets and planetary bodies. These differences represent "fossil residues" that provide invaluable insight into how the solar nebula evolved to form the planets. We cannot collect a sample of the Sun as we would for a planet; fortunately, solar material comes to us in the form of the solar wind. Ultrapure materials will be exposed at the Earth-Sun L1, outside the Earth's magnetic influence, where solar wind nuclei will be captured for 2 years before returning to Earth in January 2001. The key challenge to obtaining a good sample of solar wind, uncontaminated by terrestrial atoms, is a clean collection surface in a clean sample canister and clean facilities with which to handle the samples for allocation and future reference. The Johnson Space Center QSQ is responsible for contamination control for the mission, for ensuring the cleanliness of collection surfaces and providing a clean environment for their subsequent handling. The level of cleanliness required is high; at the time of analysis (after sample return), the surface contamination by C, N, O must each be less than 10(exp 15) atoms per centimeter squared and for elements other than C, N, O, the number of atoms per centimeter squared of each surface contaminant shall not exceed the estimated solar wind fluence of the species (varies by element between U at approx. 10 (exp 4) atoms per centimeter squared to Fe, Si, Mg, and Ne at approx. 10(exp 12), atoms per centimeter squared). Typical spacecraft assembly is done in class 10,000 cleanrooms. The final cleaning and reintegration of the Genesis payload canister as well as all sample material handling will be done within a class 10 cleanroom using Dryden suits to protect the collector materials from any human debris. Each component is unique, no standard size, shape, material, or precleaning history. We are developing new final cleaning techniques utilizing ultra-pure water to minimize molecular residues on the hardware components.

Stansbery, Eileen K.

Genesis Concentrator Target Particle Contamination Mapping and Material Identification

The majority of surface particles were found to be < 5 microns in diameter with increasing numbers close to the optical resolution limit of 0.3 microns. Acceleration grid EDS results show that the majority of materials appear to be from the SRC shell and SLA materials which include carbon-carbon fibers and Si-rich microspheres in a possible silicone binder. Other major debris material from the SRC included white paint, kapton, collector array fragments, and Al. Image analysis also revealed that SRC materials were also found mixed with the Utah mud and salt deposits. The EDS analysis of the acceleration grid showed that particles < 1 m where generally carbon based particles. Chemical cleaning techniques with Xylene and HF in an ultrasonic bath are currently being investigated for removal of small particles by the Genesis science team as well as ultra-pure water megasonic cleaning by the JSC team [4]. Removal of organic contamination from target materials is also being investigated by the science team with the use of UV-ozone cleaning devices at JSC and Open University [5]. In preparation for solar wind oxygen analyses at UCLA and Open University [1, 2], surface particle contamination on three Genesis concentrator targets was closely examined to evaluate cleaning strategies. Two silicon carbide (Genesis sample # 60001 and 60003) and one chemical vapor deposited (CVD) 13C concentrator target (60002) were imaged and mosaic mapped with optical microscopes. The resulting full target mosaic images and particle feature maps were subsequently compared with non-flight, but flight-like, concentrator targets and sample return capsule (SRC) materials. Contamination found on the flown concentrator acceleration grid was further examined using a scanning electron microscope (SEM). Energy dispersive X-ray spectroscopy (EDS) for particle identification was subsequently compared with the optical images from the flown targets. Figure 1 show that all three targets imaged in this report are fully intact and do not show any signs of material fractures. However, previous ellipsometry results and overview imaging of both flown SiC targets show a solar wind irradiation gradient from the center focal point to the outer edge [3]. In addition, due to the hard landing, each target has experienced varying degrees of impacts, scratches, and particle debris from the spacecraft and Utah impact site.

Calaway, Michael J.

Reducing Organic Contamination in NASA JSC Astromaterial Curation Facility

Future robotic and human spaceflight missions to the Moon, Mars, asteroids and comets will require handling and storing astromaterial samples with minimal inorganic and organic contamination to preserve the scientific integrity of each sample. Much was learned from the rigorous attempts to minimize and monitor organic contamination during Apollo, but it was not adequate for current analytical requirements; thus [1]. OSIRIS-REx, Hayabusa-2, and future Mars sample return will require better protocols for reducing organic contamination. Future isolation con-tainment systems for astromaterials, possibly nitrogen enriched gloveboxes, must be able to reduce organic and inorganic cross-contamination. In 2012, a baseline study established the current state of organic cleanliness in gloveboxes used by NASA JSC astromaterials curation labs that could be used as a benchmark for future mission designs [2, 3]. After standard ultra-pure water (UPW) cleaning, the majority of organic contaminates found were hydrocarbons, plasticizers, silicones, and solvents. Hydro-carbons loads (> C7) ranged from 1.9 to 11.8 ng/cm2 for TD-GC-MS wafer exposure analyses and 5.0 to 19.5 ng/L for TD-GC-MS adsorbent tube exposure. Plasticizers included < 0.6 ng/cm2 of DBP, DEP, TXIB, and DIBP. Silicones included < 0.5 ng/cm2 of cyclo(Me2SiO)x (x = 6, 8, 9, 10) and siloxane. Solvents included < 1.0 ng/cm2 of 2-cyclohexen-1-one, 3,5,5-trimethyl- (Isopho-rone), N-formylpiperidine, and 2-(2-butoxyethoxy) ethanol. In addition, DBF, rubber/polymer additive was found at < 0.2 ng/cm2 and caprolactam, nylon-6 at < 0.6 ng/cm2. Reducing Organics: The Apollo program was the last sam-ple return mission to place high-level organic requirements and biological containment protocols on a curation facility. The high vacuum complex F-201 glovebox in the Lunar Receiving Labora-tory used ethyl alcohol (190 proof), 3:1 benzene/methanol (nano grade solution), and heat sterilization at 130degC for 48 hours to reduce organic contamination. In addition, both heat sterilization and peracetic acid sterilization were used in the atmospheric de-contamination (R) cabinets. Later, Lunar curation gloveboxes were degreased with a pressurized Freon 113 wash. Today, UPW has replaced Freon as the standard cleaning procedure, but does not have the degreasing solvency power of Freon. Future Cleaning Studies: Cleaning experiments are cur-rently being orchestrated to study how to degrease and reduce organics in a JSC curation glovebox lower than the established baseline. Several new chemicals in the industry have replaced traditional degreasing solvents such as Freon and others that are now federally restricted. However, these new suites of chemicals remain untested for lowering organics in curation gloveboxes. 3M's HFE-7100DL and DuPont's Vertrel XF are currently being tested as a replacement for Freon 113 as a degreaser at JSC cura-tion facilities. In addition, the use of UPW as a final rinse is be-ing tested, which presumably can maintain a lower total organic carbon load than the filtered purity of chemical solutions. References: [1] Allton J.H. et al. (2012) LPS XLIII, 2439; [2] Calaway M.

Calaway, M. J.

Development of Genesis Solar Wind Sample Cleanliness Assessment: Initial Report on Sample 60341 Optical Imagery and Elemental Mapping

Since 2005 the Genesis science team has experimented with techniques for removing the contaminant particles and films from the collection surface of the Genesis fragments. A subset of ~40 samples have been designated as "cleaning matrix" samples. These are small samples to which various cleaning approaches are applied and then cleanliness is assessed optically, by TRXRF, SEM, ToF-SIMS, XPS, ellipsometry or other means [1-9]. Most of these sam-ples remain available for allocation, with cleanliness assessment data. This assessment allows evaluation of various cleaning techniques and handling or analytical effects. Cleaning techniques investigated by the Genesis community include acid/base etching, acetate replica peels, ion beam, and CO2 snow jet cleaning [10-16]. JSC provides surface cleaning using UV ozone exposure and ultra-pure water (UPW) [17-20]. The UPW rinse is commonly used to clean samples for handling debris between processing by different researchers. Optical microscopic images of the sample taken before and after UPW cleaning show what has been added or removed during the cleaning process.

Gonzalez, C. P.

Enhanced Cleaning of Genesis Solar Wind Sample 61348 for Film Residue Removal

The Genesis mission returned to Earth on September 8, 2004, experiencing a nonnominal reentry. During the recovery of the collector materials from the capsule, many of the collector fragments were placed on the adhesive protion of post-it notes to prevent the fragments from moving during transport back to Johnson Space Center. This unknowingly provided an additional contaminate that would prove difficult to remove with the limited chemistries allowed in the Genesis Curation Laboratory. Generally when collector material samples are prepared for allocation to PIs, the samples are cleaned front side only with Ultra-Pure Water (UPW) via megasonic dispersion to the collector surface to remove crash debris and contamination. While this cleaning method works well on samples that were not placed on post-its during recovery, it has caused movement of the residue on the back of the sample to be deposited on the front in at least two examples. Therefore, samples placed on the adhesive portion on post-it note, require enhanced cleaning methods since post-it residue has proved resistant to UPW cleaning.

Allums, K. K.

Genesis Solar Wind Sample 61422: Experiment in Variation of Sequence of Cleaning Solvent for Removing Carbon-Bearing Contamination

The recovered Genesis collector fragments are heavily contaminated with crash-derived particulate debris. However, megasonic treatment with ultra-pure-water (UPW; resistivity (is) greater than18 meg-ohm-cm) removes essentially all particulate contamination greater than 5 microns in size [e.g.1] and is thus of considerable importance. Optical imaging of Si sample 60336 revealed the presence of a large C-rich particle after UPW treatment that was not present prior to UPW. Such handling contamination is occasionally observed, but such contaminants are normally easily removed by UPW cleaning. The 60336 particle was exceptional in that, surprisingly, it was not removed by additional UPW or by hot xylene or by aqua regia treatment. It was eventually removed by treatment with NH3-H2O2. Our best interpretation of the origin of the 60336 particle was that it was adhesive from the Post-It notes used to stabilize samples for transport from Utah after the hard landing. It is possible that the insoluble nature of the 60336 particle comes from interaction of the Post-It adhesive with UPW. An occasional bit of Post-It adhesive is not a major concern, but C particulate contamination also occurs from the heat shield of the Sample Return Capsule (SRC) and this is mixed with inorganic contamination from the SRC and the Utah landing site. If UPW exposure also produced an insoluble residue from SRC C, this would be a major problem in chemical treatments to produce clean surfaces for analysis. This paper reports experiments to test whether particulate contamination was removed more easily if UPW treatment was not used.

Allton, J. H.

Genesis Solar Wind Sample Curation Facility

The controlled access facility designed and constructed for storing and examining Genesis solar wind samples consists of two adjacent laboratories, both ISO Class 4 cleanrooms (vertical laminar flow, ULPA filtered). One cleanroom is equipped with ultrapure water (UPW) for experimental cleaning of containers and tools used in handling the solar wind samples, flight hardware and witness plates. The ultrapure water is also used for cleaning the solar wind samples. The other cleanroom is for long-term nitrogen storage of samples and for examination and processing of Genesis samples.

Curation Facility

Evaluating experimental artifacts in hydrothermal prebiotic synthesis experiments

Control experiments with ultra pure deionized water were conducted to evaluate the organic contamination in hydrothermal prebiotic experiments. Different combinations of reaction vessel material, sampling tubing and stirring were tested and the amounts of organic contaminants determined. All tested types of polymer tubing were proven to introduce organic contaminants (formate, acetate and propionate ions) into the reacting solution. Stainless steel has a catalytic effect on the decomposition of formate, consistent with earlier work at high temperatures and pressures.

Equipment and Supplies

Analysis of Ultra-Pure Gases by Ion Mobility Spectrometry

Work has continued with the evaluation of the Ion Mobility Spectrometer (IMS) for the analysis of gases having low parts-per-billion (10(exp -9)) water concentration. A modified PCP, inc. MMS-160 Mobility Mass Spectrometer System was used for the analysis of ultra-pure argon and nitrogen. The MMS-160 system permits the mass-identification of unique reactant and product ions observed in the reduced-water host gases. When the water is removed to low ppb levels, higher energy reactant ions are observed. In nitrogen, distinct odd- and even-numbered nitrogen cluster ion mobility peaks are observed, as well as adduct ion peaks from the trace contaminants in the gas. Argon also produces a cluster ion mobility peak and adduct ion peaks from trace components in the gas. Levels of contaminants in these ultra-pure gases can be determined from the ion mobility spectra. A calibrated source was used to provide variable known quantities of water to the pure gas supply of the IMS.

Stimac, Robert M.

Ultra-Pure, High Endurance Liquid Bladder with Volume Sensor for Space Applications

The NASA Portable Life Support System (PLSS) for the Exploration Extravehicular Mobility Unit (xEMU) incorporates a Feedwater Supply Assembly (FSA) to store consumable cooling water. The FSA accepts pure water prior to each Extra-Vehicular Activity (EVA), then supplies this water to a membrane evaporator at ambient suit pressure during the eight hour EVA. The FSA must function reliably for hundreds of EVAs over 15 years of service without introducing contamination that may accumulate and foul the membrane. We present a unique design that combines the benefits of a flexible fluoropolymer bladder with the strength and convenience of a rigid tank, providing an ultra-pure, ambient-pressure reservoir with fill-drain cycle life exceeding 3000, internal pressure tolerance exceeding 100 psi, high volumetric efficiency, near-zero dead volume, optical transparency for visual inspection, simplified mounting, and very low mass. We also incorporate a novel volume sensor suitable for both microgravity and arbitrarily accelerated environments and capable of real-time monitoring with accuracy on the order of 2.5% full scale. Analytical predictions are supported by experimental test data from a mature subscale prototype.

PLSS Portable Life Support System FSA Feedwater Su

Isothermal Decomposition of Hydrogen Peroxide Dihydrate

We present a new method of growing pure solid hydrogen peroxide in an ultra high vacuum environment and apply it to determine thermal stability of the dihydrate compound that forms when water and hydrogen peroxide are mixed at low temperatures. Using infrared spectroscopy and thermogravimetric analysis, we quantified the isothermal decomposition of the metastable dihydrate at 151.6 K. This decomposition occurs by fractional distillation through the preferential sublimation of water, which leads to the formation of pure hydrogen peroxide. The results imply that in an astronomical environment where condensed mixtures of H2O2 and H2O are shielded from radiolytic decomposition and warmed to temperatures where sublimation is significant, highly concentrated or even pure hydrogen peroxide may form.

Loeffler, M. J.

High Energy Cutting and Stripping Utilizing Liquid Nitrogen

The Aerospace Industry has endeavored for decades to develop hybrid materials that withstand the rigors of mechanized flight both within our atmosphere and beyond. The development of these high performance materials has led to the need for environmentally friendly technologies for material re-work and removal. The NitroJet(TM) is a fluid jet technology that represents an evolution of the widely used, large-scale water jet fluid jet technology. It involves the amalgamation of fluid jet technology and cryogenics technology to create a new capability that is applicable where water jet or abrasive jet (water jet plus entrained abrasive) are not suitable or acceptable because of technical constraints such as process or materials compatibility, environmental concerns and aesthetic or legal requirements. The NitroJet(TM) uses ultra high-pressure nitrogen to cut materials, strip numerous types of coatings such as paint or powder coating, clean surfaces and profile metals. Liquid nitrogen (LN2) is used as the feed stream and is pressurized in two stages. The first stage pressurizes sub cooled LN2 to an intermediate pressure of between 15,000 and 20,000 psi at which point the temperature of the LN2 is about -250 F. The discharge from this stage is then introduced as feed to a dual intensifier system, which boosts the pressure from 15,000 - 20,000 psi up to the maximum operating pressure of 55,000 psi. A temperature of about -220 F is achieved at which point the nitrogen is supercritical. In this condition the nitrogen cuts, strips and abrades much like ultra high-pressure water would but without any residual liquid to collect, remove or be contaminated. Once the nitrogen has performed its function it harmlessly flashes back into the atmosphere as pure nitrogen gas. The system uses heat exchangers to control and modify the temperature of the various intake and discharge nitrogen streams. Since the system is hydraulically operated, discharge pressures can be easily varied over a very wide range providing considerable flexibility for various operations. The NitroJet(TM) is an advance on the nitrogen fluid jet technology initially developed at the Idaho National Engineering Laboratory in Idaho Falls, Idaho. NitroCision(R) first introduced the NitroJet(TM) into a commercial setting in 2003 and there has been considerable interest from many diverse sectors of government and industry since then. While the current system is an industrial system with the size and mass normally associated with industrial applications, a smaller system that is much more compact is being contemplated for those applications that do not need the full capabilities of the larger system. The NitroJet(TM) can be deployed as a fixed or mobile system with multiple end effectors capable of cutting, stripping, cleaning, and surface profiling either in robotic or manual applications.

Hume, Howard