Thermal analysis-inorganic gas release studies of lunar samples
Thermal analysis-quadrupole mass spectrometric analyses on inorganic released gases of Apollo 11 and 12 samples and synthetic lunar analogs
Gibson, E. K., Jr.↗
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Inorganic analysis in a controlled ecological life support system
Techniques useful for the elemental analysis of samples of types which might require analysis within a controlled ecological life support system are investigated.
Carden, J. L.↗
Techniques for the inorganic analysis in a controlled ecological life support system
Sample preparation, instrumental analysis, a direct injection device for IC/ICP interfacing, a hydraulic jet bend impaction device, monodisperse aerosol generator, and low gravity environments are discussed.
Source record↗
Some aspects of analytical chemistry as applied to water quality assurance techniques for reclaimed water: The potential use of X-ray fluorescence spectrometry for automated on-line fast real-time simultaneous multi-component analysis of inorganic pollutants in reclaimed water
The potential use of isotopically excited energy dispersive X-ray fluorescence (XRF) spectrometry for automated on line fast real time (5 to 15 minutes) simultaneous multicomponent (up to 20) trace (1 to 10 parts per billion) analysis of inorganic pollutants in reclaimed water was examined. Three anionic elements (chromium 6, arsenic and selenium) were studied. The inherent lack of sensitivity of XRF spectrometry for these elements mandates use of a preconcentration technique and various methods were examined, including: several direct and indirect evaporation methods; ion exchange membranes; selective and nonselective precipitation; and complexation processes. It is shown tha XRF spectrometry itself is well suited for automated on line quality assurance, and can provide a nondestructive (and thus sample storage and repeat analysis capabilities) and particularly convenient analytical method. Further, the use of an isotopically excited energy dispersive unit (50 mCi Cd-109 source) coupled with a suitable preconcentration process can provide sufficient sensitivity to achieve the current mandated minimum levels of detection without the need for high power X-ray generating tubes.
Ling, A. C.↗
Uncertainty evaluation in reference material characterization by double isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS)
Double isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS) is one of the most important measurement methods in the establishment of measurement standards for inorganic analysis. However, there is still no good consensus on approaches for uncertainty evaluation in double ID-ICP-MS. Particularly, approaches to treating the instrumental isotopic fractionation (IIF) phenomenon and correlation between uncertainty sources are diverse and often unclear in the literature. Here, an approach for uncertainty evaluation in double ID-ICP-MS measurements is described. Using three certified reference materials (CRMs), it is shown that the IIF effects cancel out and should not be included in the uncertainty budget. Further, a consistent way of considering correlated sources of uncertainty to prevent double counting of uncertainties is described in detail along with an example of measuring the mass fraction of magnesium in an oyster powder CRM.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Spacecraft Water Impurity Monitor, a System for Water Quality Analysis on Exploration Missions Beyond Low Earth Orbit
Exploration missions beyond low-earth-orbit (LEO) will require advanced instrumentation to monitor water quality. Traveling beyond LEO means the transfer of water samples to an Earth-based laboratory for detailed analysis is not feasible. Detailed analysis of water composition during exploration is still necessary, because having the capability to determine the specific organic chemical causing a change in total organic carbon (TOC) or the specific metal or ionic species causing a change in conductivity has the potential to inform the crew health and system management decisions. On a new vehicle such as a lunar or Mars surface habitat or a Mars transit vehicle, finding “new” impurities not seen on ISS should be expected. The key is to identify the impurity so the correct action can be taken. On ISS we can measure TOC, conductivity, and other physical properties but do not have the capability for detailed analysis using vehicle instrumentation. This is acceptable because ISS can send samples down to Earth for further analysis and obtain the detailed composition. The Spacecraft Water Impurity Monitor (SWIM) will provide detailed water quality analysis for missions in which sample down mass is not available. SWIM is a system comprising organic and inorganic analysis modules. For organic chemicals, a gas chromatograph mass spectrometer (GCMS) detects and identifies organic impurities. For inorganic species, a capillary electrophoresis capacitively coupled contactless conductivity detection (CE-C4D) system as well as ion specific electrodes detect and identify metal ions and other inorganic salts / acids. The SWIM technology demonstration project has completed a System Requirements Review (SRR) to finalize detection requirements and is currently working to refine vehicle interface requirements for a future technology demonstration. The project also has begun preliminary flight design activities for the core analyzers in the instrument suite.
Water Monitoring↗
Spacecraft Water Impurity Monitor, a System for Water Quality Analysis on Exploration Missions Beyond Low Earth Orbit
Exploration missions beyond low-earth-orbit (LEO) will require advanced instrumentation to monitor water quality. Traveling beyond LEO means the transfer of water samples to an Earth-based laboratory for detailed analysis is not feasible. Detailed analysis of water composition during exploration is still necessary, because having the capability to determine the specific organic chemical causing a change in total organic carbon (TOC) or the specific metal or ionic species causing a change in conductivity has the potential to inform the crew health and system management decisions. On a new vehicle such as a lunar or Mars surface habitat or a Mars transit vehicle, finding “new” impurities not seen on ISS should be expected. The key is to identify the impurity so the correct action can be taken. On ISS we can measure TOC, conductivity, and other physical properties but do not have the capability for detailed analysis using vehicle instrumentation. This is acceptable because ISS can send samples down to Earth for further analysis and obtain the detailed composition. The Spacecraft Water Impurity Monitor (SWIM) will provide detailed water quality analysis for missions in which sample down mass is not available. SWIM is a system comprising organic and inorganic analysis modules. For organic chemicals, a gas chromatograph mass spectrometer (GCMS) detects and identifies organic impurities. For inorganic species, a capillary electrophoresis capacitively coupled contactless conductivity detection (CE-C4D) system as well as ion specific electrodes detect and identify metal ions and other inorganic salts / acids. The SWIM technology demonstration project has completed a System Requirements Review (SRR) to finalize detection requirements and is currently working to refine vehicle interface requirements for a future technology demonstration. The project also has begun preliminary flight design activities for the core analyzers in the instrument suite.
Water Monitoring↗
The Spacecraft Water Impurity Monitor, a Framework for the Next Generation Complete Water Analysis System for Crewed Vehicles Beyond the ISS
The Spacecraft Water Impurity Monitor (SWIM) is a joint collaboration to develop an instrument platform that will perform in-flight measurements and deliver a more complete picture of water quality to decision makers. Eventually, missions to the moon, Mars, and beyond will be equipped with analytical capabilities equaling those found in terrestrial labs. Based on what we know about current and future spacecraft environments, SWIM will seek to provide enhanced analytical capability that enables NASA to confidently send astronauts on distant missions without the possibility of returned water samples. This paper discusses the challenges presented by exploration requirements and the research and development progress toward the goal of a total water analysis system. For organic analysis, one of the analysis technologies that the SWIM team have been developing is a liquid-injection gas chromatograph mass spectrometer system; these systems are the workhorses of analytical chemistry laboratories world-wide. For inorganic analysis, the team is exploring a number of technologies ranging from traditional liquid chromatography technologies (e.g. ion chromatography, capillary electrophoresis) to flight-heritage technology such as ion-specific electrodes.
water monitoring↗
Viking survey paper
The paper reviews Viking injection into Mars orbit, the landing, and the Orbiter. The following Viking investigations are discussed: the search for life (photosynthetic analysis, metabolic analysis, and respiration), molecular analysis, inorganic chemistry, water detection, thermal mapping, radio science, and physical and seismic characteristics. Also considered are the imaging system, the lander camera, entry science, and Mars weather.
Soffen, G.↗
Development of biological and nonbiological explanations for the Viking label release data
The plausibility that hydrogen peroxide, widely distributed within the Mars surface material, was responsible for the evocative response obtained by the Viking Labeled Release (LR) experiment on Mars was investigated. Although a mixture of gamma Fe2O3 and silica sand stimulated the LR nutrient reaction with hydrogen peroxide and reduced the rate of hydrogen decomposition under various storage conditions, the Mars analog soil prepared by the Viking Inorganic Analysis Team to match the Mars analytical data does not cause such effects. Nor is adequate resistance to UV irradiation shown. On the basis of the results and consideration presented while the hydrogen peroxide theory remains the most, if not only, attractive chemical explanation of the LR data, it remains unconvincing on critical points. Until problems concerning the formation and stabilization of hydrogen peroxide on the surface of Mars can be overcome, adhere to the scientific evidence requires serious consideration of the biological theory.
Source record↗
Viking magnetic properties experiment - Extended mission results
The backhoe magnets on Viking Lander (VL) 2 were successfully cleaned, followed by a test involving successive insertions of the cleaned backhoe into the surface. Rapid saturation of the magnets confirmed evidence from primary mission results that the magnetic mineral in the Martian surface is widely distributed, most probably in the form of composite particles of magnetic and nonmagnetic minerals. An image of the VL 2 backhoe taken via the X4 magnifying mirror demonstrates the fine-grained nature of the attracted magnetic material. The presence of maghemite and its occurrence as a pigment in, or a thin coating on, all mineral particles or as discrete, finely divided and widely distributed crystallites, are consistent with data from the inorganic analysis experiments and with laboratory simulations of results of the biology experiments on Mars.
Hargraves, R. B.↗
A search for a nonbiological explanation of the Viking Labeled Release life detection experiment
The possibility of nonbiological reactions involving hydrogen peroxide being the source of the positive response detected by the Viking Labeled Release (LR) life detection experiment on the surface of Mars is assessed. Labeled release experiments were conducted in the LR Test Standards Module which replicates the Viking flight instrument configuration on analog Martian soils prepared to match the Viking inorganic analysis of Mars surface material to which an aqueous solution of hydrogen peroxide had been added. Getter experiments were also conducted to compare several reactions simultaneously in the presence and absence of UV radiation prior to the addition of nutrient. Hydrogen peroxide on certain analog soils is found to be capable of reproducing the kinetics and thermal information contained in the Mars data. The peroxide concentration necessary for this response, however, is shown to require a chemical stability or production rate much greater than seems likely in the Mars environment. As previous experiments have shown hydrogen peroxide to be the most likely nonbiological source of the positive LR response, it is concluded that the presence of a biological agent on Mars must not yet be ruled out.
Levin, G. V.↗
Analysis and interpretation of Viking inorganic chemistry data (Mars data analysis program)
Soil samples gathered by the Viking Lander from the surface of Mars were analyzed. The Martian fines were lower in aluminum, iron, sulfur, and chlorine than typical terrestrial continental soils or lunar mare fines. Sample variabilities were as great within a few meters as between lander locations (4500 km apart) implying the existence of a universal Martian regolith component of constant average composition.
Clark, B. C.↗
Mars, clays and the origins of life
To detect life in the Martian soil, tests were designed to look for respiration and photosynthesis. Both tests (labeled release, LR, and pyrolytic release, PR) for life in the Martian soils were positive. However, when the measurement for organic molecules in the soil of Mars was made, none were found. The interpretation given is that the inorganic constituents of the soil of Mars were responsible for these observations. The inorganic analysis of the soil was best fitted by a mixture of minerals: 60 to 80 percent clay, iron oxide, quartz, and soluble salts such as halite (NaCl). The minerals most successful in simulating the PR and LR experiments are iron-rich clays. There is a theory that considers clays as the first organisms capable of replication, mutation, and catalysis, and hence of evolving. Clays are formed when liquid water causes the weathering of rocks. The distribution of ions such as aluminum, magnesium, and iron play the role of bases in the DNA. The information was stored in the distribution of ions in the octahedral and tetrahedral molecules, but that they could, like RNA and DNA, replicate. When the clays replicated, each sheet of clay would be a template for a new sheet. The ion substitutions in one clay sheet would give rise to a complementary or similar pattern on the clay synthesized on its surface. It was theorized that it was on the surface of replicating iron-rich clays that carbon dioxide would be fixed in the light into organic acids such as formic or oxalic acid. If Mars had liquid water during a warm period in its past, clay formation would have been abundant. These clays would have replicated and evolved until the liquid water was removed due to cooling of Mars. It is entirely possible that the Viking mission detected life on Mars, but it was clay life that awaits the return of water to continue its evolution into life based on organic molecules.
Hartman, Hyman↗
Preparation of Ion Exchange Films for Solid-Phase Spectrophotometry and Solid-Phase Fluorometry
Atomic spectroscopy has dominated the field of trace inorganic analysis because of its high sensitivity and selectivity. The advantages gained by the atomic spectroscopies come with the disadvantage of expensive and often complicated instrumentation. Solid-phase spectroscopy, in which the analyte is preconcentrated on a solid medium followed by conventional spectrophotometry or fluorometry, requires less expensive instrumentation and has considerable sensitivity and selectivity. The sensitivity gains come from preconcentration and the use of chromophore (or fluorophore) developers and the selectivity is achieved by use of ion exchange conditions that favor the analyte in combination with speciative chromophores. Little work has been done to optimize the ion exchange medium (IEM) associated with these techniques. In this report we present a method for making ion exchange polymer films, which considerably simplify the solid-phase spectroscopic techniques. The polymer consists of formaldehyde-crosslinked polyvinyl alcohol with polyacrylic acid entrapped therein. The films are a carboxylate weak cation exchanger in the calcium form. They are mechanically sturdy and optically transparent in the ultraviolet and visible portion of the spectrum, which makes them suitable for spectrophotometry and fluorometry.
Hill, Carol M.↗
Analysis of the Organic and Inorganic Constituents of Carbonaceous and Other Selected Stony Meteorites Semiannual Status Report, 1 Nov. 1965 - 1 May 1966
Chemical analysis of organic and inorganic constituents of carbonaceous and other stony meteorites
CARBONACEOUS METEORITE↗
Understanding the impacts of inorganic species in woody biomass for preprocessing and pyrolysis–A review
Woody biomass represents an abundant resource for sustainable biofuels, biochemicals, and bioproducts. Technologies for converting woody biomass have been established for decades, and research consistently highlights the critical role of inorganic species and ash plays in feedstock handling and conversion processes, including equipment plugging, corrosion, and catalyst deactivation. A thorough understanding of the variability, transport behavior, and downstream impact of inorganic species in woody biomass is essential for defining feedstock quality specifications and developing effective management strategies for conversion processes. This review compiles critical information in five main sections: 1) inorganic species concentration in woody biomass, based on anatomical fractions and their sources of variability; 2) technique features for quantifying inorganic elemental chemical analysis; 3) impacts of inorganic species on biomass preprocessing; 4) impacts of inorganic species on pyrolysis, and 5) mitigation strategies. Additionally, this review explores future challenges and opportunities in addressing the impacts of inorganic species on biomass quality. These insights aim to support the sustainable development of the biomass-to-bioenergy pipeline and ensure high-quality lignocellulosic feedstocks for efficient downstream conversions. The findings offer valuable guidance to policy makers, industry stakeholders, and researchers in developing effective strategies for managing inorganic species in woody biomass and fostering the sustainable processes for lignocellulosic biorefineries.
09 BIOMASS FUELS↗
Inorganic chemical investigation by X-ray fluorescence analysis - The Viking Mars Lander
The inorganic chemical investigation experiment added in August 1972 to the Viking Lander scientific package uses an energy-dispersive X-ray fluorescence spectrometer in which four sealed, gas-filled proportional counters detect X-rays emitted from samples of the Martian surface materials irradiated by X-rays from radioisotope sources (Fe-55 and Cd-109). The instrument is inside the Lander body, and samples are to be delivered to it by the Viking Lander Surface Sampler. Instrument design is described along with details of the data processing and analysis procedures. The results of the investigation will characterize the surface materials of Mars as to elemental composition with accuracies ranging from a few tens of parts per million (at the trace-element level) to a few per cent (for major elements) depending on the element in question.
Toulmin, P., III↗