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All sourcesNASA NTRSDOE OSTI
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Implications of Deep UV Raman Spectra of Gypsum and Fe-Bearing Dust Mixtures for Gypsum Detectability by the SHERLOC M2020 Instrument

Key science objectives of the Mars2020 Scanning Habitable Environments with Raman & Luminescence for Organics & Chemicals (SHERLOC) instrument suite include identification and characterization of inorganic and bio-logic phases and investigation of the past habitability of Jezero crater [1, 2]. To fully interpret in situ data received from SHERLOC, databases of deep ultraviolet (DUV) Raman spectra from a wide variety of martian analogue materials are being developed by us and others [e.g., 3]. Ferrous and ferric iron are abundant on the martian surface in bas-alt and, depending on alteration and transport processes, its alteration products. Fe-bearing phases are important to characterize with respect to detect-ability by DUV Raman spectroscopy because they strongly absorb DUV radiation, thereby decreasing Raman peak intensity [3, 4]. Ca-sulfates and Fe-bearing minerals have been commonly detected on the martian surface [5, 6]. In this analogue study, we collected Raman spectra of mechanical mixtures of powders of hematite HMS3 (~120 nm discrete particle diameter [7]), palagonite HWMK919 (<5 μm size fraction [8]) and gypsum WD163 (<150 μm size fraction) t o ex-amine the detectability of gypsum in the presence of relatively finer-grained, Fe bearing material. Be-cause of the difference in particle diameters, hematite and palagonite powders act as surrogates for martian dust, coating at small concentrations and then enveloping larger gypsum particles.

N C Haney↗
NASA NTRS2011

Experimental Shock Transformation of Gypsum to Anhydrite: A New Low Pressure Regime Shock Indicator

The shock behavior of gypsum is important in understanding the Cretaceous/Paleogene event and other terrestrial impacts that contain evaporite sediments in their targets (e.g., Mars Exploration Rover Spirit detected sulfate at Gusev crater, [1]). Most interest focuses on issues of devolatilization to quantify the production of SO2 to better understand its role in generating a temporary atmosphere and its effects on climate and biota [2,3]. Kondo and Ahrens [4] measured induced radiation emitted from single crystal gypsum shocked to 30 and 40 GPa. They observed greybody emission spectra corresponding to temperatures in the range of 3,000 to 4,000 K that are a factor of 2 to 10 times greater than calculated pressure-density energy equation of state temperatures (Hugoniot) and are high enough to melt gypsum. Chen et al. [5] reported results of shock experiments on anhydrite, gypsum, and mixtures of these phases with silica. Their observations indicated little or no devolatilization of anhydrite shocked to 42 GPa and that the fraction of sulfur, by mass, that degassed is approx.10(exp -2) of theoretical prediction. In another report of shock experiments on calcite, anhydrite, and gypsum, Badjukov et al. [6] observed only intensive plastic deformation in anhydrite shock loaded at 63 GPa, and gypsum converted to anhydrite when shock loaded at 56 GPa but have not experimentally shocked gypsum in a step-wise manner to constrain possible incipient transformation effects. Schmitt and Hornemann [7] shock loaded anhydrite and quartz to a peak pressure of 60 GPa and report the platy anhydrite grains were completely pseudomorphed by small crystallized anhydrite grains. However, no evidence of interaction between the two phases could be observed and they suggested that recrystallization of anhydrite grains is the result of a solid-state transformation. They concluded that significant decomposition of anhydrite requires shock pressures higher than 60 GPa. Gupta et al. [8] reanalyzed the calcite and anhydrite shock wave experiments of Yang [9] using improved equations of state of porous materials and vaporized products. They determined the pressures for incipient and complete vaporization to be 32.5 and 122 GPa for anhydrite GPa which is a factor of 2 to 3 lower than reported earlier by Yang [9]. These studies are not in agreement regarding the onset of sulfate decomposition and documentation of shock effects in gypsum is incomplete.

Bell, Mary S.↗
DOE OSTI2023

ADVANCED TECHNIQUES FOR ENERGY INPUT REDUCTION IN GYPSUM WALLBOARD DRYING

Gypsum has been used for thousands of years in building and construction applications, starting with the pyramids in ancient Egypt, to “Plaster of Paris” in the midcenturies, and to the now-ubiquitous drywall in modern-day houses. Production of gypsum drywall boards takes several steps with high energy and water consumption. The current state of the art in industry is a process that begins by mining gypsum and reducing its particle size by milling. These gypsum particles undergo calcination to convert the gypsum (calcium sulfate dihydrate) into stucco (calcium sulfate hemihydrate). The stucco is mixed with additives and enough water to form a slurry that can be poured onto a conveyor belt and molded into the desired geometry. The stucco reacts with the water, converting back into gypsum. The remaining water is then dried from the board to form the final product. While only ~20 wt. % of water is needed for the conversion of stucco to gypsum, significant excess water is needed to ensure sufficient fluidity of the slurry for processibility. This is due to the low quality of the stucco particles produced in high throughput calcination units, which disintegrate upon mixing with water, thereby reducing the fluidity and processability of the slurry. This project aims to produce high-quality stucco particles by dielectric calcination. In doing so, particle integrity can be maintained through the slurry formulation step, and particle size distribution of the stucco can be adjusted to increase fluidity with less excess water. With less water remaining unreacted in the board, significant energy can be saved in drying the product. The project aims to 1) develop a dielectric calcination method to TRL 3, 2) determine optimal and practical particle size distributions to minimize excess water in the slurry, and 3) reduce the energy consumption of the drying process.

Conforti, Kameron↗
DOE OSTI2025

Microbial ecology of acidic, biogenic gypsum: community structure and distribution of extremophiles on freshly formed and relict sulfate deposits in a hydrogen sulfide-rich cave

Sulfate minerals are abundant on the Martian surface, and many of these evaporite deposits are thought to have precipitated from acidic fluids. On Earth, gypsum (CaSO 4 •2H 2 O) and other sulfates sometimes form under acidic conditions, so exploring the extremophilic life that occurs in these mineral environments can help evaluate the astrobiological potential of acid sulfate depositional settings. Here, we characterized the microbial communities associated with acidic gypsum deposits in a sulfuric acid cave, where sulfate precipitation is driven by sulfide-oxidizing bacteria and archaea. We used 16S rRNA gene sequencing and cell counts to characterize gypsum-associated microorganisms in freshly formed and relict deposits throughout the cave, to test how microbial community composition and abundance would vary with distance from the sulfidic water table and with the concentration of H 2 S(g) and other gases in the cave atmosphere. We found that actively forming gypsum in the lower cave levels was colonized by low-diversity communities that have few cells compared to other environments in the cave. The most abundant taxa were Acidithiobacillus, Metallibacterium, Mycobacteria, and three different Thermoplasmatales-group archaea, which occupied distinct niches based on proximity to sulfidic streams and the concentration of gases in the cave air. By contrast, deposits in older cave levels had more diverse communities that were distinct from those associated with freshly formed gypsum and likely represent a community reliant on different energy resources. These findings show that acidic sulfate deposits serve as habitats for extremophilic microorganisms and broaden our knowledge of the life associated with terrestrial sulfates.

58 GEOSCIENCES↗
NASA NTRS1992

Albedo patterns and gypsum generation in the central Namib Desert - Land, sea and air interactions on an arid West Coast

In the central Namib Desert, dune-free surfaces are separated abruptly from a sea of yellow and red sand dunes at the Kuiseb River canyon. The off-white hues of the dune-free area result from anomalously high surficial gypsum enrichment. Satellite imagery indicates that the gypsum surfaces are associated with lower surface maximum temperatures than those of the darker dune surfaces to the south. One of various sources of sulfate for the gypsum bodies is oceanic H2S, supplied to desert land-surfaces by regular fog incursions. Since fog events are widespread along the coast, the question of anomalous gypsum accumulations north of the dune sea arises. Satellite imagery, in conjunction with more detailed handheld photography from the space shuttle, indicates that the penetration of fog inland is significantly greater over the gypsum surfaces than it is over the dunes. It is postulated that the thermal gradient between these surfaces generates a heat low centered over the northern part of dune sea and that this enhances fog and H2S advection on its north side onto the nearby dune-free zone. In such a system, gypsum/caliche surfaces reinforce advection of fog over themselves in a positive feedback mode.

Wilkinson, M. J.↗
DOE OSTI2025

Thermal and mechanical performance of gypsum composites containing fly ash cenosphere encapsulated phase change materials

Utilizing phase change materials (PCMs) within construction materials improves the thermal energy storage capabilities in the built environment. Notably, integrating PCMs into drywalls presents a promising avenue to reduce building energy use. However, incorporating PCMs into drywalls poses challenges, particularly reduced mechanical properties and workability limitations as it can adversely affect the hardening and cohesiveness of gypsum composites. To address these challenges, this study explores a novel strategy to incorporate PCMs into gypsum composites through fly ash cenosphere-encapsulated PCM, namely CenoPCM, aiming to enhance the mechanical properties and thermal conductivity over existing commercial counterparts. An experimental program was conducted to study the impact of the inclusion of CenoPCM on the mechanical and thermal performance of gypsum composites, and the results were compared to those of commercially available polymerencapsulated PCM benchmark (Micronal). The findings highlighted that PCM-charged samples exhibited up to 95.90 J/g (CenoPCM) of latent heat with 70 % CenoPCM loading. The results of mechanical tests also showed that CenoPCM outperformed its polymer-encapsulated counterpart, achieving 55 % higher mechanical strength on average. Here, this improvement is attributed to the rigid shell of fly ash cenosphere (FAC) serving as a PCM carrier, providing a skeleton-like structure to gypsum composites for higher load-bearing capacity. Additionally, hotbox tests demonstrated that the CenoPCM-charged wall panels yielded a 20 % higher thermal conductivity and a 22 % increased time lag compared to Micronal PCM-charged panels, indicating its potential to shift the peak load in buildings.

Ceno PCM↗
DOE OSTI2022

Bassanite Grows Along Distinct Coexisting Pathways and Provides a Low Energy Interface for Gypsum Nucleation

Calcium sulfate is a naturally abundant and industrially important mineral; understanding its formation mechanism contributes to reconstructing geochemical record and controlling its scaling in industry. Formation of gypsum is shown to follow a multistage-processes via bassanite, but the evolution of bassanite and the mechanism by which it is replaced by gypsum are poorly understood. Here we outline a three-stage process: (i) growth of bassanite nanoparticles into nanorods or rosettes, (ii) extension of bassanite rosettes by addition of fundamental growth units and aggregation of bassanite nanorods into aggregates, and (iii) heterogeneous nucleation of gypsum on the tips of bassanite rosettes and aggregates. The findings demonstrate that bassanite grows via distinct coexisting pathways and provides a low energy interface for heterogeneous nucleation of gypsum, thus providing proofs that more than one growth pathway can operate simultaneously in a crystallization system and that the precursors in multistage crystallization processes can imprint their pattern of precipitation onto the final phase.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Impact of Electromagnetic Fields on Gypsum and Silica Scaling in Reverse Osmosis

Electromagnetic field (EMF) is a cost-effective, simple, and energy-efficient method for scale control in reverse osmosis (RO) systems. However, its effects on gypsum and silica scaling, as well as the underlying mechanisms, remain poorly understood. This study systematically investigates the effects of EMF treatment on gypsum and silica scaling in RO systems, utilizing synthetic brackish water and natural RO concentrate (ROC) from a desalination facility. For gypsum, EMF changes the crystal morphology, resulting in the formation of a porous, less compact scaling layer. It is more readily removed through hydraulic flushing (HF), enhancing scaling reversibility and water recovery. In the case of silica scaling, EMF promotes homogeneous polymerization in the bulk solution, producing larger silica particles that inhibit the formation of a dense, cross-linked gel layer on the membrane surface, mitigating flux decline. This study thus demonstrates EMF’s effectiveness in controlling gypsum scaling in undersaturated feedwaters when combined with HF and in mitigating silica scaling under both HF and non-HF conditions for supersaturated feedwaters. These findings underscore EMF’s versatility as a nonchemical approach for scale control in RO desalination and show its substantial potential to enhance membrane performance and operational efficiency in real-world water treatment applications.

Du, Xuewei [New Mexico State University, Las Cruce↗
NASA NTRS2009

Relative Shock Effects in Mixed Powders of Calcite, Gypsum, and Quartz: A Calibration Scheme from Shock Experiments

The shock behavior of calcite and gypsum is important in understanding the Cretaceous/Tertiary event and other terrestrial impacts that contain evaporite sediments in their targets. Most interest focuses on issues of devolatilization to quantify the production of CO2 or SO2 to better understand their role in generating a temporary atmosphere and its effects on climate and biota [e.g., papers in 1,2,3,4]. Devolatilization of carbonate is also important because the dispersion and fragmentation of ejecta is strongly controlled by the expansion of large volumes of gas during the impact process as well [5,6]. Shock recovery experiments for calcite yield seemingly conflicting results: early experimental devolatilization studies [7,8,9] suggested that calcite was substantially outgassed at 30 GPa (> 50%). However, the recent petrographic work of [10,11,12] presented evidence that essentially intact calcite is recovered from 60 GPa experiments. [13] reported results of shock experiments on anhydrite, gypsum, and mixtures of those phases with silica. Their observations indicate little or no devolatilization of anhydrite shocked to 42 GPa and that the fraction of sulfur, by mass, that degassed is approx.10(exp -2) of theoretical prediction. In another (preliminary) report of shock experiments on calcite, anhydrite, and gypsum, [14] observe calcite recrystallization when shock loaded at 61 GPa, only intensive plastic deformation in anhydrite shock loaded at 63 GPa, and gypsum converted to anhydrite when shock loaded at 56 GPa. [15] shock loaded anhydrite and quartz to a peak pressure of 60 GPa. All of the quartz grains were trans-formed to glass and the platy anhydrite grains were completely pseudomorphed by small crystallized anhydrite grains. However, no evidence of interaction between the two phases could be observed and they suggest that recrystallization of anhydrite grains is the result of a solid state transformation. [16] reanalyzed the calcite and anhydrite shock wave experiments of [17] using improved equations of state of porous materials and vaporized products. They determined the pressures for incipient and complete vaporization to be 32.5 and 122 GPa for anhydrite and 17.8 and 54.1 GPa for calcite, respectively, a factor of 2 to 3 lower than reported earlier by [17].

Bell, Mary S.↗
DOE OSTI2026

Discovery of nanopore filling by gypsum in wellbore cement exposed to 17 MPa CO 2 under geologic carbon storage conditions

Here, this study investigates the pore structure evolution of the reaction zones in wellbore cement samples exposed to a CO 2 -rich solution in equilibrium with 17 MPa supercritical CO 2 over 14 days. Through advanced characterization methods of field emission SEM, Quantitative Evaluation of Minerals by Scanning Electron Microscopy (QEMSCAN), and micro-CT, a new mechanism of CO 2 -cement reaction involving filling of nanopores in the interior of cement by gypsum was revealed. Gypsum was formed by the liberation of SO 4 2− from ettringite (AFt) and monosulfate (AFm) caused by a decrease in pH. Based on these experimental observations, a new CO 2 -cement reaction model that incorporates four distinct reaction zones is developed. This model provides a comprehensive framework for understanding the spatial and temporal distribution of minerals in cement due to high pressure CO 2 —cement reactions. This study demonstrates that the major damage induced by high pressure CO 2 alteration occurs in the most exterior region of the cement. The interior region of the cement maintains its integrity due to nanopore filling by gypsum.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS1980

Friction evaluation of unpaved, gypsum-surface runways at Northrup Strip, White Sands Missile Range, in support of Space Shuttle Orbiter landing and retrieval operations

Friction measurement results obtained on the gypsum surface runways at Northrup Strip, White Sands Missile Range, N. M., using an instrumented tire test vehicle and a diagonal braked vehicle, are presented. These runways were prepared to serve as backup landing and retrieval sites to the primary sites located at Dryden Flight Research Center for shuttle orbiter during initial test flights. Similar friction data obtained on paved and other unpaved surfaces was shown for comparison and to indicate that the friction capability measured on the dry gypsum surface runways is sufficient for operations with the shuttle orbiter and the Boeing 747 aircraft. Based on these ground vehicle friction measurements, estimates of shuttle orbiter and aircraft tire friction performance are presented and discussed. General observations concerning the gypsum surface characteristics are also included and several recommendations are made for improving and maintaining adequate surface friction capabilities prior to the first shuttle orbiter landing.

Yager, T. J.↗
NASA NTRS2012

Comparison of Four Strong Acids on the Precipitation Potential of Gypsum in Brines During Distillation of Pretreated, Augmented Urine

In this study, three different mineral acids were substituted for sulfuric acid (H2SO4) in the urine stabilizer solution to eliminate the excess of sulfate ions in pretreated urine and assess the impact on maximum water recovery to avoid precipitation of minerals during distillation. The study evaluated replacing 98% sulfuric acid with 85% phosphoric acid (H3PO4), 37% hydrochloric acid (HCl), or 70% nitric acid (HNO3). The effect of lowering the oxidizer concentration in the pretreatment formulation also was studied. This paper summarizes the test results, defines candidate formulations for further study, and specifies the injection masses required to stabilize urine and minimize the risk of mineral precipitation during distillation. In the first test with a brine ersatz acidified with different acids, the solubility of calcium in gypsum saturated solutions was measured. The solubility of gypsum was doubled in the brines acidified with the alternative acids compared to sulfuric acid. In a second series of tests, the alternative acid pretreatment concentrations were effective at preventing precipitation of gypsum and other minerals up to 85% water recovery from 95th-percentile pretreated, augmented urine. Based on test results, phosphoric acid is recommended as the safest alternative to sulfuric acid. It also is recommended that the injected mass concentration of chromium trioxide solution be reduced by 75% to minimize liquid resupply mass by about 50%, reduce toxicity of brines, and reduce the concentration of organic acids in distillate. The new stabilizer solution formulations and required doses to stabilize urine and prevent precipitation of minerals up to 85% water recovery are given. The formulations in this study were tested on a limited number of artificially augmented urine batches collected from employees at the Johnson Space Center (JSC). This study successfully demonstrated that the desired physical and chemical stability of pretreated urine and brines can be achieved using alternate pretreatment formulations under laboratory conditions. Additional testing and hazard assessments will be required to determine the feasibility of utilizing the proposed urine pretreatment formulations on ISS.

Muirhead, Dean↗
DOE OSTI2023

Novel ammonia recovery from anaerobic digestion by integrating biogas stripping and gypsum absorption

Recovering ammonia from anaerobic digestion (AD) effluent offers the opportunity to produce a renewablefertilizer and reduce environmental impact. A novel process developed for such an application was evaluatedduring this study. The feature of the process is integrating biogas stripping and gypsum (CaSO 4 •2H 2 O) absorption. The result revealed that the lower CO 2 content and the absorption temperature contributed the higherefficiency of ammonia recovery. The gypsum solution recovered around 95% of the stripped ammonia when thestripping gas contained 10% CO 2 and it rose to 100% when the gas contained more than 30% CO 2 . Furthermore,a statistical model and genetic algorithm were applied to estimate the total ammonia recovery and optimize theoperating parameters. The experimental and modeling results indicated that integrating biogas stripping withgypsum absorption can effectively harvest ammonia nitrogen and reduce CO 2 emissions while producing(NH 4 ) 2 SO 4 fertilizer from AD effluent.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Radio Frequency Calcination of Gypsum for Sustainable Wallboard Production

This presentation details several accomplishments in the dielectric calcination of gypsum to stucco. 1) Verification that gypsum can be calcined via RF heating, 2)Characterization of heating and mass loss curve for a nucleation propagation reaction under electromagnetics 3) Full parametric studies examining effect of free moisture on heating and calcination, and 4) Finite element model of process with high predictive capability. Overall, Industrial implementation could save up to 63% energy, 50% water, and reduce carbon emissions by 63% based on batch scale studies.

Tjards, Jacob↗
DOE OSTI2024

Influence of zwitterionic amphiphilic copolymers on heterogeneous gypsum formation: A promising approach for scaling resistance

Here, this study aims to investigate the influence of zwitterionic amphiphilic copolymers (ZACs) in the nucleation and growth of heterogeneous CaSO4 at the zwitterion-water interface, which is crucial for the prevention of mineral scaling and consequent downtime or suboptimal performance in industries like membrane desalination, heat exchangers, and pipeline transportation. In situ grazing incidence small angle X-ray Scattering (GISAXS), and quartz crystal microbalance with dissipation (QCM-D) techniques were used to analyze the evolution of CaSO 4 particles on two new ZAC coatings: poly-(trifluoroethyl methacrylate-random-sulfobetaine methacrylate) (PTFEMA-r-SBMA, or PT:SBMA) and poly(trifluoroethyl methacrylate-random-2-methacryloyloxyethyl phosphorylcholine) (PTFEMA-r-MPC, or PT:MPC). The results showed that PT:MPC coatings promoted nucleation but inhibited crystal growth, resulting in slower overall reaction kinetics on PT:MPC coatings compared to PT:SBMA coatings. Interfacial interactions involving the substrates, sulfate minerals, and ions were examined, revealing that calcium ion adsorption, primarily governed by electrostatic attraction, played a crucial role in the nucleation and growth processes on both ZAC coatings. The crystal characterization revealed a phase transition from bassanite to gypsum on both ZAC coatings, suggesting that these zwitterionic materials can influence the mineral phase of heterogeneously formed CaSO 4 crystals. These findings enhance our understanding of the fundamental mechanisms underlying heterogeneous CaSO 4 scaling in the presence of zwitterionic materials.

42 ENGINEERING↗
DOE OSTI2024

Gypsum and clay-based additives to MSW for pre-combustion enhancement of syngas and solid residue improvement (Final Scientific/Technical Report)

This project was focused on the development of a cost-effective and practical approach for the recovery of metals and syngas from municipal solid waste (MSW) thermally processed in a gasification or combustion (i.e. waste-to-energy (WTE)) facility with the inclusion of other waste streams. The goal of additional waste inclusion was targeted to change the oxidation of critical and precious elements to enable them to be more efficiently recovered. The project had two main components: laboratory testing and techno-economic analysis (TEA). The additional waste included with MSW as gypsum and spent FCC (sFCC) catalyst as additives to improve material recovery and energy efficiency in MSW and WTE ash.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Structural evolution of amorphous calcium sulfate nanoparticles into crystalline gypsum phase

The involvement of amorphous calcium sulfate (ACS) as a precursor to calcium sulfate crystallization remains an important but poorly understood phenomenon, especially the mechanism by which ACS evolves into crystalline phase. In this study, we captured the ACS nanoparticles as a precursor to calcium sulfate crystallization in a concentrated CaCl 2 solution at 90 °C and observed several stages of its evolution. The ACS nanoparticles grew by simultaneous fusion and internal structural evolution. Aggregation of the ACS nanoparticles gave birth to bulk ACS particles within which nanocrystalline domains sprouted and developed into crystalline gypsum. This work deepens the understanding of the evolution of ACS nanoparticles and its role in multistage crystallization of calcium sulfate.

36 MATERIALS SCIENCE↗