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Results for “differential scanning calorimeter”

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At least 19 records

Phoenix Lander's Thermal Evolved Gas Analyzer: Differential Scanning Calorimeter and Mass Spectrometer Database Development

The Mars Scout Phoenix lander will land in the north polar region of Mars in May, 2008. One objective of the Phoenix lander is to search for evidence of past life in the form of molecular organics that may be preserved in the subsurface soil. The Thermal Evolved Gas Analyzer (TEGA) was developed to detect these organics by coupling a simultaneous differential thermal analyzer (SDTA) with a mass spectrometer. Martian soil will be heated to approx.1000 C and potential organic decomposition products such as CO2, CH4 etc. will be examined for with the MS. TEGA s SDTA will also assess the presence of endothermic and exothermic reactions that are characteristic of soil organics and minerals as the soil is heated. The MS in addition to detecting organic decompositon products, will also assess the levels of soil inorganic volatiles such as H2O, SO2, and CO2. Organic detection has a high priority for this mission; however, TEGA has the ability to provide valuable insight into the mineralogical composition of the soil. The overall goal of this work is to develop a TEGA database of minerals that will serve as a reference for the interpretation of Phoenix-TEGA. Previous databases for the ill-fated Mars Polar Lander (MPL)-TEGA instrument only went to 725 C. Furthermore, the MPL-TEGA could only detect CO2 and H2O while the Phoenix-TEGA MS can examine up to 144 atomic mass units. The higher temperature Phoenix-TEGA SDTA coupled with the more capable MS indicates that a higher temperature database is required for TEGA interpretation. The overall goal of this work is to develop a differential scanning calorimeter (DSC) database of minerals along with corresponding MS data of evolved gases that can used to interpret TEGA data during and after mission operations. While SDTA and DSC measurement techniques are slightly different (SDTA does not use a reference pan), the results are fundamentally similar and thus DSC is a useful technique in providing comparative data for the TEGA database. The objectives of this work is to conduct DSC and MS analysis up to 1000 C of select minerals that may be found in the martian soil.

Sutter, B.↗

New eutectic alloys and their heats of transformation

Eutectic compositions and congruently melting intermetallic compounds in binary and multicomponent systems among common elements such as Al, Ca, Cu, Mg, P, Si, and Zn may be useful for high temperature heat storage. In this work, heats of fusion of new multicomponent eutectics and intermetallic phases are reported, some of which are competitive with molten salts in heat storage density at high temperatures. The method used to determine unknown eutectic compositions combined results of differential thermal analysis, metallography, and microprobe analysis. The method allows determination of eutectic compositions in no more than three steps. The heats of fusion of the alloys were measured using commercial calorimeters, a differential thermal analyzer, and a differential scanning calorimeter.

Farkas, D.↗

Investigations Using Laboratory Testbeds to Interpret Flight Instrument Datasets from Mars Robotic Missions

The Astromaterials Research and Exploration Science Directorate at the NASA Johnson Space Center (JSC) has laboratory instrumentation that mimic the capabilities of corresponding flight instruments to enable interpretation of datasets returned from Mars robotic missions. The lab instruments have been and continue to be applied to datasets for the Moessbauer Spectrometer (MB) on the Mars Exploration Rovers (MER), the Thermal & Evolved Gas Analyzer (TEGA) on the Mars Phoenix Scout, the CRISM instrument on the Mars Reconnaissance Orbiter Missions and will be applied to datasets for the Sample Analysis at Mars (SAM), Chemistry and Mineralogy (CheMin) and Chemistry & Camera (ChemCam) instruments onboard the Mars Science Laboratory (MSL). The laboratory instruments can analyze analog samples at costs that are substantially lower than engineering models of flight instruments, but their success to enable interpretation of flight data depends on how closely their capabilities mimic those of the flight instrument. The JSC lab MB instruments are equivalent to the MER instruments except without flight qualified components and no reference channel Co-57 source. Data from analog samples were critical for identification of Mg-Fe carbonate at Gusev crater. Fiber-optic VNIR spectrometers are used to obtain CRISM-like spectral data over the range 350-2500 nm, and data for Fephyllosilicates show irreversible behavior in the electronic transition region upon dessication. The MB and VNIR instruments can be operated within chambers where, for example, the absolute H2O concentration can be measured and controlled. Phoenix's TEGA consisted of a calorimeter coupled to a mass spectrometer (MS). The JSC laboratory testbed instrument consisted of a differential scanning calorimeter (DSC) coupled to a MS configured to operate under total pressure (12 mbar), heating rate (20 C/min), and purge gas composition (N2) analogous to the flight TEGA. TEGA detected CO2 release at both low (400-680 C) and high (725-820 C) temperature and an endothermic reaction in concert with the high temperature release. The high-temperature thermal decomposition is consistent with calcite, dolomite, or ankerite, (3-6 wt.%) or any combination of these phase based upon laboratory testbed experiments. Recent laboratory experiments suggest that the low temperature CO2 release was caused by a reaction between calcium carbonate and hydrated magnesium perchlorate; although, CO2 release by the oxidation of organic materials and Fe-/Mg-rich carbonates cannot be ruled out. MSL landed in Gale crater on August 5, 2012. Although numerous analog samples have been analyzed on the JSC laboratory testbeds, no SAM, CheMin, or ChemCam analyses have been acquired by MSL to date. The JSC SAM laboratory testbed consists of a thermal analyzer coupled with a MS configured to operate under total pressure (30 mbar), heating rate (35 C/min), and purge gas composition (He) analogous to the flight SAM. The CheMin and ChemCam laboratory testbeds were developed and built by inXitu, Inc. and Los Alamos National Laboratory, respectively, to acquire datasets relevant to the MSL CheMin and ChemCam flight instruments.

Ming, D. W.↗

The comet rendezvous asteroid flyby mission

The Comet Rendezvous Asteroid Flyby Mission (CRAF) is described. After gravity assists from Venus and Earth, the spacecraft will fly by the asteroid 46 Hestia en route to a rendezvous with P/Tempel 2 in Nov. 1996, when the comet is near aphelion. The scientific experiments for the CRAF mission are: an imaging system; a visual and infrared mapping spectrometer; an infrared radiometer; a penetrator carrying a gamma-ray spectrometer, a scanning differential calorimeter and evolved gas analyzer, accelerometers, and temperature probes; a neutral gas and thermal ion mass spectrometer; a secondary ion mass spectrometer for analyzing dust, gas, and thermal ions; a scanning electron microscope and particle analyzer; an X-ray fluorescence and gas chromatographic analyzer for collected dust and ice samples; a dust counter and velocity analyzer; a retarding potential ion mass spectrometer; a supra-thermal ion mass spectrometer and electron analyzer; a magnetometer; and a coordinated radio, electron, and plasma wave analyzer.

Neugebauer, M.↗

Irradiation effects in rapidly and conventionally solidified alloys. Phase stability in rapidly solidified N i-Nb under Ni ion irradiation

Two alloy compositions in the Ni-Nb system (Ni60Nb40 and Ni85Nb15) were produced by rapidly quenching from the melt with the piston anvil technique. The Ni60Nb40 was transformed to a metastable, partially crystalline state by heat treatment in a differential scanning calorimeter. The Ni85Nb15 was fully crystalline, with the majority of the grains composed of collections of primary dendrite arms. Both compositions were irradiated with 4 MeV Ni++ ions. The irradiation induced microstructures were examined by transmission electron microscopy and compared with thermally aged samples. The thermal evolution was arrested by ion irradiation in the temperature range studied, by inhibiting the nucleation of the NiNb phase. No irradiation induced voids were observed. It is found that the ion irradiation drives the microstructure along a different path than thermal evolution.

Source record↗

Planetary exploration sensor systems

Most of the instruments that have been used in planetary exploration have been either spectrometers or imaging devices. Instruments of these types are being developed for the Galileo and VOIR (Venus Orbiting Imaging Radar) missions. Galileo will take advantage of new CCD (charge-coupled device) technology, and VOIR will use techniques of synthetic aperture radar developed for Seasat. For determining the macrostructure of mineral resources, the best approach is believed to involve acoustic imaging, essentially a seismic data processing technique. Determinations of microstructure would require a light microscope and an electron microscope. For determining the nature and form of volatiles, a differential scanning calorimeter could be used. To determine the mineral composition, an electron beam microprobe with X-ray fluorescence and spectroscopy would be used.

Saunders, R. S.↗

An Evaluation of Techroll Seal Flexible Joint Material

This study evaluated the materials utilized in the flexible joint for possible failure modes. Studies undertaken included effect of temperature on the strength of the system, effect of fatigue on the strength of the system, thermogravimetric analysis, thermochemical analysis, differential scanning calorimeter analysis, dynamic mechanical analysis, and peel test. These studies indicate that if the joint failed due to a materials deficiency, the most likely mode was excessive temperature in the joint. In addition, the joint material is susceptible to fatigue damage which could have been a contributing factor.

Hall, W. B.↗

Materials testing of the IUS techroll seal material

As a part of the investigation of the control system failure Inertial Upper Stage on IUS-1 flight to position a Tracking and Data Relay Satellite (TDRS) in geosynchronous orbit, the materials utilized in the techroll seal are evaluated for possible failure models. Studies undertaken included effect of temperature on the strength of the system, effect of fatigue on the strength of the system, thermogravimetric analysis, thermomechanical analysis, differential scanning calorimeter analysis, dynamic mechanical analysis, and peel test. The most likely failure mode is excessive temperature in the seal. In addition, the seal material is susceptible to fatigue damage which could be a contributing factor.

Nichols, R. L.↗

Kinetics of crystal nucleation and growth in Pd(40)Ni(40)P(20) glass

Samples of Pd(40)Ni(40)P(20) glass, produced by cooling the melt at 1 or 800 K/s, are heated in a differential scanning calorimeter to determine the crystallization kinetics. Optical microscopy shows that eutectic crystallization proceeds both by growth from the surface of the samples and by the growth of spherical regions around preexisting nuclei in the interior. A modified Kissinger (1957) analysis is used to obtain the activation energy for crystal growth (3.49 eV). The steady state homogeneous nucleation frequency at 590 K is about 10 million/cu m per sec. This is estimated to be the maximum nucleation frequency: it is too low to account for the observed population of quenched-in nuclei, which are therefore presumed to be heterogeneous. The major practical obstacle to glass formation in this system is heterogeneous nucleation.

Drehman, A. J.↗

Aircraft Safety Improvement

Fabrication and testing of honeycomb sandwich aircraft panels are discussed. Also described is the use of the following instruments: thermogravimetric analyzer, differential scanning calorimeter, limiting oxygen index, and infrared spectrometer.

Kao, G.↗

Non-isothermal crystallization of poly(etheretherketone) aromatic polymer composite

The nonisothermal crystallization kinetics of PEEK APC-2 and of 450G neat resin PEEK material were compared using a differential scanning calorimeter to monitor heat flow during crystallization; the effects of cooling rate on the crystallization temperature, the degree of crystallinity, and the conversion rate were investigated. A modified Avrami (1940) analysis was used to describe nonisothermal crystallization kinetics. It was found that, compared with the 450G neat resin PEEK, the nonisothermal crystallization of the PEEK APC-2 composite is characterized by higher initiation temperature, higher heat flow maximum temperature, and greater relative conversion by primary processes.

Cebe, Peggy↗

Design of a sample acquistion system for the Mars exobiological penetrator

The Mars Exobiological Penetrator will be imbedded into several locations on the Martian surface. It contains various scientific instruments, such as an Alpha-Particle Instrument (API), Differential Scanning Calorimeter (DSC), Evolved Gas Analyzer (EGA) and accelerometers. A sample is required for analysis in the API and DSC. To avoid impact contaminated material, this sample must be taken from soil greater than 2 cm away from the penetrator shell. This study examines the design of a dedicated sampling system including deployment, suspension, fore/after body coupling, sample gathering and placement. To prevent subsurface material from entering the penetrator sampling compartment during impact, a plug is placed in the exit hole of the wall. A U-lever device is used to hold this plug in the penetrator wall. The U-lever rotates upon initial motion of the core-grinder mechanism (CGM), releasing the plug. Research points to a combination of coring and grinding as a plausible solution to the problem of dry drilling. The CGM, driven by two compressed springs, will be deployed along a tracking system. A slowly varying load i.e., springs, is favored over a fixed displacement motion because of its adaptability to different material hardness. However, to accommodate sampling in a low density soil, two dash pots set a maximum transverse velocity. In addition, minimal power use is achieved by unidirectional motion of the CGM. The sample will be transported to the scientific instruments by means of a sample placement tray that is driven by a compressed spring to avoid unnecessary power usage. This paper also explores possible modifications for size, weight, and time as well as possible future studies.

Thomson, Ron↗

Two Radiative/Thermochemical Instruments

Measurements of absorption and emission complement thermal measurements. Two laboratory instruments for research in combustion and pyrolysis equipped for radiative as well as thermal measurements. One instrument essentially differential scanning calorimeter (DSC) modified to detect radiation emitted by flames. Provides means to evaluate limits of flammability of materials exhibiting exothermic reactions in DSC's. Other instrument used to determine pyrolysis properties of specimens exposed to various gases by measurement of infrared absorption spectra of pyrolysis products.

Tapphorn, Ralph M.↗

Characterizing water/rock interaction in simulated comet nuclei via calorimetry: Tool for in-situ science, laboratory analysis, and sample preservation

Although results from the Giotto and Vega spacecraft flybys of comet P/Halley indicate a complex chemistry for both the ices and dust in the nucleus, carbonaceous chondrite meteorites are still regarded as useful analogs for the rocky components. Carbonaceous chondrites mixed with water enable simulation of water/rock interactions which may occur in cometary nuclei. Three general types of interactions can be expected between water and minerals at sub-freezing temperatures: heterogeneous nucleation of ice by insoluble minerals; adsorption of water vapor by hygroscopic phases; and freezing and melting point depression of liquid water sustained by soluble minerals. Two series of experiments were performed in a differential scanning calorimeter (DSC) with homogenized powders of the following whole-rock meteorites and comparison samples: Allende (CV3), Murchison (CM2), Orgueil (CI), Holbrook (L6), and Pasamonte (eucrite) meteorites as well as on peridotite (PCC-1, USGS), saponite (Sap-Ca-1, CMS), montmorillonite (STx-1, CMS), and serpentine (Franciscan Formation, California). Results are briefly discussed.

Allton, Judith H.↗

The oxygen sensitivity/compatibility ranking of several materials by different test methods

Eleven materials were evaluated for oxygen compatibility using the following test methods: heat of combustion (ASTM D 2015), liquid oxygen impact (ASTM D 2512), pneumatic impact (ASTM G 74), gaseous mechanical impact (ASTM G 86), autogenous ignition temperature by pressurized differential scanning calorimeter, and the determination of the 50 percent reaction level in liquid oxygen using silicon carbide as a reaction enhancer. The eleven materials evaluated were: Teflon TFE, Vespel SP-21, Krytox 240AC, Viton PLV5010B, Fluorel E2160, Kel F 81, Fluorogold, Fluorogreen E-600, Rulon A, Garlock 8573, nylon 6/6.

Lockhart, Billy J.↗

Thermal Analyzer for Planetary Soil (TAPS): an in Situ Instrument for Mineral and Volatile-element Measurements

Thermal Analyzer for Planetary Soil (TAPS) offers a specific implementation for the generic thermal analyzer/evolved-gas analyzer (TA/EGA) function included in the Mars Environmental Survey (MESUR) strawman payload; applications to asteroids and comets are also possible. The baseline TAPS is a single-sample differential scanning calorimeter (DSC), backed by a capacitive-polymer humidity sensor, with an integrated sampling mechanism. After placement on a planetary surface, TAPS acquires 10-50 mg of soil or sediment and heats the sample from ambient temperature to 1000-1300 K. During heating, DSC data are taken for the solid and evolved gases are swept past the water sensor. Through ground based data analysis, multicomponent DSC data are deconvolved and correlated with the water release profile to quantitatively determine the types and relative proportions of volatile-bearing minerals such as clays and other hydrates, carbonates, and nitrates. The rapid-response humidity sensors also achieve quantitative analysis of total water. After conclusion of soil-analysis operations, the humidity sensors become available for meteorology. The baseline design fits within a circular-cylindrical volume less than 1000 cm(sup 3), occupies 1.2 kg mass, and consumes about 2 Whr of power per analysis. Enhanced designs would acquire and analyze multiple samples and employ additional microchemical sensors for analysis of CO2, SO2, NO(x), and other gaseous species. Atmospheric pumps are also being considered as alternatives to pressurized purge gas.

Gooding, J. L.↗

Fusible heat sink materials - Evaluation of alternate candidates

Fusible heat sinks are a possible source for thermal regulation of space suited astronauts. Materials with greater thermal storage capability than water could enable both an extension of time between recharging and/or a reduction in size and/or mass. An extensive literature search identified 1,215 candidates with a solid-liquid transformation within the temperature range of -13 C to 5 C. Based on data available in the literature, several candidates with a cooling capacity significantly greater than water were identified. Measurements of the transformation temperature and enthalpy of transformation were then undertaken with a differential scanning calorimeter in order to confirm the accuracy of the literature. Laboratory measurements have thus far not been able to corroborate the extremely high values found from the literature. This paper presents the approach for materials selection utilized in this study, the experimental procedure, and the results of the measurements thus far undertaken.

Selvaduray, Guna S.↗