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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Investigation of Lubricant Additive Interactions on Gasoline Particulate Filters

To understand how the composition of novel lubricant additives and their ash interact with gasoline particulate filters (GPFs), an accelerated aging protocol was conducted using three lubricant additive formulations and two GPF types. The additive packages (adpaks) consisted of Ca+Mg detergent in a 3:1 or 0:1 ratio and an anti-wear component—either zinc dialkyl dithiophosphate (ZDDP) or a novel phosphonium-phosphinate ionic liquid (IL) substitute. The particulate sampling captured amount/compositions of particulate matter (PM) generated, total particulate number, and size distribution. Five ash loadings were completed. GPF position and adpak composition affected the backpressure, ash composition, ash morphology, and captured mass. The particulate sampling indicated that the ash component consisted primarily of particles less than 50 nm in size and that the Mg-only adpak resulted in more particulate of 50–400 nm in size. Postmortem materials characterization indicated GPFs in the underfloor position had deeper penetration of ash into the walls compared to the close-coupled position. Additionally, the Mg-only adpak had a higher filter collection efficiency (>90%) and the ash particles consisted of a higher concentration of dense ash material. In contrast, four of the 3:1 Ca:Mg lubricant adpaks resulted in a collection efficiency of only 40–50%. Although the collection efficiency was higher with the Mg-only adpak, the ash layer in the GPF was not thicker, nor was the penetration into the wall more significant, and surprisingly the full useful life (FUL) backpressure was lower than with Ca:Mg adpaks. The higher density of the Mg-derived ash was the only detectable difference. A possible explanation of this observation is that Mg ash has a lower melting point and is more susceptible to densification during combustion or GPF regeneration. The substitution of IL in place of the ZDDP did not lead to any notable changes in collection efficiency or location of the ash.

42 ENGINEERING↗
DOE OSTI2015

Removal of introduced inorganic content from chipped forest residues via air classification

Inorganic content in biomass decreases the efficiency of conversion processes, especially thermochemical conversions. The combined concentrations of specific ash forming elements are the primary attributes that cause pine residues to be considered a degraded energy conversion feedstock, as compared to clean pine. Air classification is a potentially effective and economical tool to isolate high inorganic content biomass fractions away from primary feedstock sources to reduce their ash content. In this work, loblolly pine forest residues were air classified into 10 fractions whose ash content and composition were measured. Ash concentrations were highest in the lightest fractions (5.8–8.5 wt%), and in a heavy fraction of the fines (8.9–15.1 wt%). The removal of fractions with high inorganic content resulted in a substantial reduction in the ash content of the remaining biomass in forest thinnings (1.69–1.07 wt%) and logging residues (1.09–0.68 wt%). These high inorganic content fractions from both forest residue types represented less than 7.0 wt% of the total biomass, yet they contained greater than 40% of the ash content by mass. Elemental analysis of the air classified fractions revealed the lightest fractions were comprised of high concentrations of soil elements (silicon, aluminum, iron, sodium, and titanium). However, the elements of biological origin including calcium, potassium, magnesium, sulfur, manganese, and phosphorous were evenly distributed throughout all air classified fractions, making them more difficult to isolate into fractions with high mineral concentrations. Under the conditions reported in this study, an economic analysis revealed air classification could be used for ash removal for as little as $2.23 per ton of product biomass. As a result, this study suggests air classification is a potentially attractive technology for the removal of introduced soil minerals from pine forest residues.

09 BIOMASS FUELS↗
NASA NTRS1993

Carbon in weathered ordinary chondrites from Roosevelt County

A suite of Roosevelt County ordinary chondrites of known terrestrial age have been analyzed for carbon content and isotopic composition. Initial results indicate that significant carbon contamination is evident only in samples with a terrestrial age greater than 40 ka. These samples are of weathering grade D and E and contain three times more carbon than the less weathered samples. The soil in which they were preserved has a carbon content of ca. 1.5 percent. Over 200 meteorites have been recovered from a series of soil depleted areas of New Mexico and West Texas. Most have been recovered from blowouts near Clovis in Roosevelt County (RC) on the high plains of New Mexico. The mineralogical and petrologic Al effects of weathering upon these samples have been studied previously and show that the degree of weathering is largely depend ant upon the terrestrial residence time. The study was undertaken to determine the effects of prolonged exposure to the soil and climate of Roosevelt County upon ordinary chondrites in the hope that this will enable a better understanding of the problems associated with the collection of meteoritic falls. A suite of ten grade 4 to 6 H, L, and LL ordinary chondrites were analyzed for carbon content and isotopic composition.

Ash, R. D.↗
DOE OSTI2016

Microstructure and wear characterization of aluminum matrix composites reinforced with industrial waste fly ash particulates synthesized by friction stir processing

Fly ash (FA) is a waste product of coal combustion in thermal power plants which is available in massive quantities all over the world causing land pollution. This paper reports the characterization of AA6061 aluminum matrix composites (AMCs) reinforced with FA particles synthesized using friction stir processing (FSP). The volume fraction of FA particles was varied from 0 to 18 in steps of 6. The prepared AMCs were characterized using optical microscopy (OM), scanning electron microscopy (SEM) and electron backscattered diagram (EBSD). The wear rate was estimated using a pin-on-disc wear apparatus. FA particles were observed to be distributed homogeneously in the AMC irrespective of the location within the stir zone. The EBSD micrographs revealed remarkable grain refinement in the AMC. The incorporation of FA particles enhanced the microhardness and wear resistance of the AMC. The strengthening mechanisms of the AMC were discussed and correlated to the observed microstructures. The wear mechanisms were identified by characterizing the wear debris and worn surfaces. - Highlights: •Industrial waste fly ash was used to produce aluminum matrix composites. •Friction stir processing was used to produce AA6061/Fly Ash composite. •Fly ash particles refined the grains of aluminum matrix. •Fly ash particles enhanced the hardness and wear resistance. •Successful utilization of fly ash to make aluminum composites reduces land pollution.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Characterization of Arsenic and Selenium in Coal Fly Ash to Improve Evaluations for Disposal and Reuse Potential (Final Technical Report)

Coal fly ash is a high volume waste material that is discarded in landfills and surface water impoundments across the U.S. and is also widely recycled for a variety of applications. The leaching of potential of contaminants of concern, such as arsenic (As) and selenium (Se), is often the driver of risk assessments for coal ash disposal and reuse. The extent of leachable As and Se depends on several factors related to environmental conditions and fly ash characteristics. Previous studies employed various methods to delineate the concentration, chemical form, and distribution of As and Se in fly ash materials. However, few studies have attempted to directly correlate these properties to mobilization parameters relevant to disposal and reuse. Instead, the coal residuals industries often rely upon standardized leaching protocols that can be laborious or involve hazardous chemicals. The goals of the project were to: 1) Develop and evaluate a characterization protocol that can be used to screen fly ash samples for leachability of As and Se; 2) Characterize As, Se, and associated constituents of fly ash particles at multiple length scales (nanometer to micrometer) to determine if elemental associations differ as a function of the resolution of characterization; and 3) Establish a predictive model for the chemical composition of coal ash produced annually at major U.S. coal fired power facilities on 50-year national coal supply records. For the first objective, we performed leaching experiments with 52 fly ash samples collected from 15 different U.S. power plants and representing coal feedstocks from the three major domestic coal regions. For this work, we assessed the mobilization potential of As and Se in fly ash based on standardized leaching protocols and performed multivariate and lasso regression analyses to explore correlations of leachable As and Se contents with characteristics such as major element contents, loss on ignition (LOI) and pH. The results of regression models indicated that major elements (Fe, Ca, Al) for a wide range of fly ashes can serve as predictor variables for the leaching potential of As, but not for Se. LOI and pH were not important predictive variables in the models. Both regression approaches resulted in relatively strong fits for leachable As (correlation coefficient R 2 = 0.78 for both models) compared to models for leachable Se (R 2 = 0.49). Overall, these results suggest that correlation models combined with on-site elemental analysis with portable analyzers may enable a screening method for leachable As in coal ash. For the second objective, we utilized nanoscale 2-D imaging (30-50 nm spot size) with the Hard X-ray Nanoprobe (HXN) in combination with microprobe X-ray capabilities (~5 µm resolution) to determine As and Se elemental associations in fly ash particles. Speciation of As and Se was also measured at the nano- to microscale with X-ray absorption spectroscopy. The enhanced resolution of HXN showed As and Se that were diffusely located around or comingled with Ca- and Fe-rich particles. The results also showed nanoparticles of Se attached to the surface of fly ash grains. Overall, a comparison of As and Se species across scales highlights the heterogeneity and complexity of chemical associations for these trace elements of concern in coal fly ash. For the final objective, we developed a predictive model for major element composition of coal ash in reserve at disposal sites of major U.S. coal fired power plants. This model was constructed from coal purchase records of 705 power stations from 1973-2022 and was trained on coal ash composition data showing that coal ash elemental composition is strongly associated with the source of feedstock coal. The model showed regional shifts in the major element contents of ash produced by power plants in the last 50 years, particularly for calcium and iron (expressed as %CaO and %Fe 2 O 3 ), as coal-fired power stations changed their source of coal over this time frame. Our approach enables an estimation of coal ash chemical composition that is stored in waste impoundments at individual power stations. Such information can help delineate the regional market potential for material applications that would utilize coal ash harvested from disposal sites across the U.S.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2020

Influence of 73 Rb on the ashes of accreting neutron stars

We find that the proton separation energy, S(p), of 73 Rb is –640(40) keV, deduced from the observation of β-delayed ground-state protons following the decay of 73 Sr. This lower-limit determination of the proton separation energy of 73 Rb coupled with previous upper limits from nonobservation, provides a full constraint on the mass excess with ΔM ( 73 Rb) = –46.01 ± 0.04 MeV. With this new mass excess and the excitation energy of the J π = 5/2 – isobaric-analog state (T = 3/2) in 73 Rb, an improved constraint can be put on the mass excess of 73Sr using the isobaric-multiplet mass equation (IMME), and we find ΔM( 73 Sr) = –31.98 ± 0.37 MeV. Furthermore, these new data were then used to study the composition of ashes on accreting neutron stars following Type I x-ray bursts. Counterintuitively, we find that there should be an enhanced fraction of A > 102 nuclei with more negative proton separation energies at the 72 Kr rp-process waiting point. Larger impurities of heavier nuclei in the ashes of accreting neutron stars will impact the cooling models for such astrophysical scenarios.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2023

Rapid AI-based Dissection of Ashes using Raman and XRF Spectroscopy (RADAR-X)

Waste-to-energy (WTE) facilities incinerate ~35 million tons of municipal solid waste annually in the United States. The incineration process reduces the mass and the volume of the waste fraction by over 75 and 95%, respectively. The fraction left after incineration remains as ash residues and is referred to as WTE ash, compromising of bottom and fly ash. In the United States, ~10 million tons of WTE ashes are generated annually and predominantly landfilled because of the lack of secondary end-use pathways. This incurs a significant financial burden (landfilling costs) on U.S. WTE facilities and also results in the loss of materials to the landfill. The primary objective of this research is to understand better the elemental and mineralogical composition of WTE ashes from diverse origins and find composition dependent upcycling pathways for diverting these ashes from landfills. This primary objective was addressed through three research tasks –(Task I) An AI-led Multi-Modal Approach for Compositional Analysis, (Task II) Developing a Dissolution-Based Test for Real Time Analysis, and (Task III) Establishing composition-dependent end uses. The chemical composition of WTE ash is dependent on two factors, i.e., the input waste composition and the operational parameters of a WTE facility (combustion conditions). Amongst these two factors, the input waste composition will likely show spatial and temporal variation. As a result, the chemical composition of WTE ash will also fluctuate. To understand the spatial and temporal variation in WTE ash composition, in Task I, we collected 128 ash samples (62 bottom ash and 66 fly ash samples) from 11 WTE facilities located in 11 U.S. states and characterized them via X-ray Fluorescence, powder X-ray Diffraction, and Raman Spectroscopy. The findings from this extensive characterization work indicated that the key elements in WTE fly ashes are Ca, Cl (greater than 10 wt. %), Si, S, K, Zn ( between 1 and 10 wt. %), Mg, Al, P, Ti, Fe, Cu, Br, and Pb (between 0.1 and 1 wt. %). Similarly, the key elements in WTE bottom ash fraction finer than 45μm are Ca (greater than 10 wt. %), Mg, Al, Si, S, Cl, K, Ti, Fe, Zn (between 1 and 10 wt. %), P, V, Cr, Mn, Cu, Br, and Pb (between 0.1 and 1 wt. %). Here, we note that the dominant fraction of WTE bottom ash is the coarse fraction. The coarse WTE bottom ash fraction (rich in silicon) was not characterized in this study because of excessive grinding requirements and their unsuitability as a supplementary cementitious material due to their coarse nature. The elements in WTE bottom ashes are present as calcite, anhydrite, vaterite, hydroxyapatite, quartz, bassanite, gehlenite, akermanite, hydrocalumite, and portlandite. Similarly, the mineralogical species present in WTE fly ashes are calcium chloride hydroxide, halite, calcite, anhydrite, sylvite, hydrocalumite, vaterite, hannebachite, quartz, and bassanite. Temporal variation in ash composition may also result in significant fluctuations in chemical compositions. Therefore, a WTE facility may need to monitor the ash composition (elemental and mineralogical composition) in real time. In Task I, we evaluated the possibility of using a portable X-ray fluorescence (XRF) spectrometer to monitor the elemental composition in real-time. Specifically, we collected XRF data on identical specimens via a portable XRF spectrometer (low-end) and a lab-based benchtop XRF spectrometer (high-end). The collected data was used to train an A.I. algorithm (portable XRF data as an input and benchtop XRF data as an output) to predict accurate elemental composition using portable XRF data. Finally, we developed a 2-minute photobleaching protocol to monitor the mineralogical characteristics of WTE ashes via Raman spectroscopy. Overall, the activities in Task I improved our understanding of ash composition and developed techniques to monitor elemental and mineralogical composition in near real-time. Based on the findings of Task I, we find that WTE ashes exhibit wide variability in mineralogy. For ICP-based elemental analysis, all the mineralogical species in WTE ashes must be brought into solution. This is traditionally accomplished with acid digestion using a combination of multiple acids. However, acid digestion with multiple acids is time-consuming and often fails to ensure complete digestion of the ash matrix. To address this limitation, in Task II, we developed an alkali-fusion-based digestion protocol using a combination of lithium tetraborate, lithium metaborate, and their combinations as possible alkali fluxes for digesting WTE ashes entirely and rapidly. The validity of the developed method was evaluated on two standard ash specimens, i.e., SRM 1633c coal fly ash and BCR-176R incineration fly ash specimen. The findings suggest that the developed protocol can ensure complete digestion of elements such as Al, Ba, Ca, Cr, Cu, Mg, Mn, P, Sr, V, Zn, Be, K, and rare earth elements. The recent changes in the energy market towards renewables and increased metal recycling have resulted in reduced supplies of supplementary cementitious materials (coal fly ash and slag). Therefore, in Task III, we evaluated the possibility of employing WTE ashes as SCMs. As the chemical composition of WTE ashes varies temporally (on an hourly basis), there was also a need to develop tests that can evaluate the suitability of material to act as supplementary cementitious material rapidly, i.e., in a few minutes. Therefore, in Task II, we also developed a rapid test to assess the suitability of a material to act as an SCM in 5 minutes. This represents a significant advance over the state-of-the-art R 3 test, which takes ~144 hours. This test was initially validated on amorphous aluminosilicates, such as calcined clays, and could be extended to evaluate other industrial by-products, such as WTE ashes. In Task III, we evaluated the possibility of employing WTE ashes for two applications, i.e., as an SCM and a lime substitute for clay stabilization. The findings from Task I indicated that WTE ashes are enriched in chlorine and, therefore, cannot be used directly as an SCM due to corrosion-related risks and altered hydration kinetics. Accordingly, we developed an ash treatment protocol to reduce the solubility of chlorine-containing species in WTE ashes. The developed treatment protocol also immobilized lead in certain mineral forms. As a result of the treatment, WTE ashes can be used as SCMs without any corrosion or heavy metal leaching concerns. The second application examined in this study was clay stabilization. WTE ashes are calcium-rich and can be an adequate lime replacement for clay stabilization. Our findings reveal that the sum of the concentrations of Ca(OH) 2 and CaClOH controls the clay stabilization capability of WTE ashes. In summary, in this work, we evaluated the elemental and mineralogical characteristics of U.S. WTE ashes from diverse origins and developed tests to evaluate the chemical characteristics of these ashes in real time through a portable XRF and a benchtop Raman spectrometer. Based on the chemical characteristics of these ashes, we developed an ash treatment process to enable the use of WTE ashes as an SCM and also evaluated the possibility of employing these ashes for clay stabilization. Overall, the findings from this work enables the diversion of WTE ashes from landfills for multiple end-uses, i.e., as an SCM or a lime substitute for clay stabilization.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Crosslinked Polyacrylamide Composite Hydrogels Impregnated with Fly Ash: Synthesis, Characterization and Their Application as Fractures Sealant for High Water Producing Zones in Oil and Gas Wells

Polymeric hydrogels are designed to serve many purposes in various fields of human endeavor. Herein, crosslinked polyacrylamide (PAM) composite hydrogels impregnated with coal fly ash (CFA) were synthesized, characterized and tested as fracture sealing agents in high water producing permeable zones in petroleum industry. The concept of utilizing CFA as an inorganic additive in the matrix of hydrogel emanates from the fact that CFA constitutes majorly alumina and silica. Both chemical oxides can induce the CFA to promote the inherent properties of hydrogel. Polyethyleneimine (PEI) was chosen as the crosslinking agent. Neat PAM/PEI hydrogel and PAM/PEI–CFA hydrogels at various CFA loadings (0.5, 1 and 2 wt%) were synthesized via a transamidation reaction pathway. The developed hydrogels were characterized by hybrid rheometer, FTIR, SEM and XRD instruments. Rheological results reveal that the PAM/PEI–CFA composite hydrogels embedded with various CFA quantities were more elastic than the neat PAM/PEI hydrogel, indicating the dispersion and reinforcing effect of CFA. The functional groups of these hydrogels were confirmed by the FTIR while SEM analysis show that the surface micrographs of neat PAM/PEI hydrogel and PAM/PEI–CFA1 hydrogel were porous in several regions. In contrast, the micrographs of PAM/PEI–CFA2 and PAM/PEI–CFA3 hydrogels demonstrated dense and “net-like” structural patterns. Further, XRD analysis revealed that CFA impregnation has a significant effect on the bulk structural properties of the fabricated hydrogels. The swelling rates of these hydrogels were determined by the gravimetric method and their diffusion parameters evaluated using Fickian diffusion and Schott-order kinetic models. Efficacy of the PAM/PEI–CFA composite hydrogel as fractures sealant in oil and gas wells was conducted at a typical reservoir temperature, 90 °C, and the outcome demonstrated considerable sealing potency.

36 MATERIALS SCIENCE↗
DOE OSTI2016

High thermal behavior of a new glass ceramic developed from silica xerogel/SnO{sub 2} composite

In this investigation, a new glass ceramics have been produced by mixing SnO{sub 2} and amorphous silica xerogel (ASX) extracted from sago waste ash. The composition has been prepared by adding 10 mol% of SnO{sub 2} into SX. The samples have been dry pressed and sintered in the temperature range between 800 °C and 1500 °C. The effects of temperature on the crystallization of silica xerogel after adding SnO{sub 2} and their relationship to bulk density have been studied. The crystallization process of the silica xerogel/SnO{sub 2} composite has been examined by an X-ray diffraction (XRD) and the bulk density has been characterized on the basis of the experimental data obtained using Archimedes′ principle. It has been found that an addition of SnO{sub 2} confers an appreciable effect on the grain and from the interpretation of XRD patterns allow one to explain the increase in the density by an increased crystallite size of SnO{sub 2} in the composite.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Properties of mortars made by uncalcined FGD gypsum-fly ash-ground granulated blast furnace slag composite binder

Highlights: Black-Right-Pointing-Pointer The mortar with uncalcined FGD gypsum has suitable workability. Black-Right-Pointing-Pointer The strength of mortar with uncalcined FGD gypsum is higher than that of mortar without uncalcined FGD gypsum. Black-Right-Pointing-Pointer The dry shrinkage of mortar with uncalcined FGD gypsum is lower than that of mortar without uncalcined FGD gypsum. Black-Right-Pointing-Pointer The leaching of sulfate ion of mortar is studied. - Abstract: A series of novel mortars were developed from composite binder of uncalcined FGD gypsum, fly ash (FA) and ground granulated blast furnace slag (GGBFS) for the good utilization of flue gas desulphurization (FGD) gypsum. At a fixed ratio (20%) of GGBFS to the composite binder, keeping consistency of the mortar between 9.5 and 10.0 cm, the properties of the composite mortar were studied. The results show that higher water/binder (W/B) is required to keep the consistency when increasing the percentage of FGD gypsum. No obvious influences of the W/B and content of FGD gypsum on the bleeding of paste were observed which keeps lower than 2% under all experimental conditions tried. The highest compressive and flexural strengths (ratio is 20% FGD gypsum, 20% GGBFS and 60% FA) are 22.6 and 4.3 MPa at 28 days, respectively. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) results indicate that massive ettringite crystals and C-S-H gels exist in the hydration products. At 90 days the mortars with FGD gypsum is dramatically smaller drying shrinkage (563-938 micro strain) than that without FGD gypsum (about 2250 micro strain). The release of the SO{sub 4}{sup 2-} from the mortar was analyzed, indicating that the dissolution of sulfate increases with FGD gypsum. The concentration of SO{sub 4}{sup 2-} releasing from the mortar with 10% FGD gypsum is almost equal to that obtained from the mortar without FGD gypsum. The release of SO{sub 4}{sup 2-} from the mortar with 20% FGD gypsum is 9200 mg{center_dot}m{sup -2}, which is lower than that from the mortar with 95% cement clinker and 5% FGD gypsum.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2019

Self-healing, re-adhering, and carbon-steel corrosion mitigating properties of fly ash-containing calcium aluminum phosphate cement composite at 300 °C hydrothermal temperature

This study assesses here the ability of calcium aluminate phosphate (CAP)/fly ash F (FAF) blend composite to self-heal at early age; to re-adhere to the casing surfaces after debonding and to protect carbon steel (CS) against brine-caused corrosion before and after the re-adherence. The composite was damaged after autoclaving for 24 h at 300 °C and then exposed to the same conditions for 5 more days for the self-healing and re-adhering processes. The ability of the blend to self-heal and re-adhere to CS was evaluated 1) by measurements of the recovery of compressive and bond strengths and Young's modulus; 2) by performing the 3-dimensional micro-image analysis of sealed cracks; 3) by phase identification in composite matrix and in the cracks after the healing; 4) by measurements of CS corrosion impediment by the re-adhered composite after 300°C-5-day restoration period. After the healing, the two factors, sealing effect of cracks by reaction products and change in phase composition of cement matrix, essentially governed the recovery of the original mechanical strength. For the former, analcime phase derived from pozzolanic FAF autogenous healing aid played the major role in sealing the cracks, while the well-formed hydroxyapatite phase contributed to the latter factor. The lap-shear bond with the strength of 1.11 MPa at CS plate/composite adhesive/CS plate joint failed cohesively, showing higher bond strength than strength of the composite matrix. The rebonded composite-CS plates developed a 0.37 MPa bond strength after the 5-day restoration period. The results of electrochemical polarization corrosion tests revealed that the re-adhered composite covering CS plate significantly inhibited the brine-caused corrosion of CS, leading to 0.011 mm/year corrosion rate, corresponding to 50% reduction compared with that of before re-adhering. There were two factors governing such corrosion mitigation: enhanced adhesive contact of composite with CS and increased coverage by the re-adhering composite.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Effects Of Crystallographic Properties On The Ice Nucleation Properties Of Volcanic Ash Particles

Specific chemical and physical properties of volcanic ash particles that could affect their ability to induce ice formation are poorly understood. In this study, the ice nucleating properties of size-selected volcanic ash and mineral dust particles in relation to their surface chemistry and crystalline structure at temperatures ranging from –30 to –38 °C were investigated in deposition mode. Ice nucleation efficiency of dust particles was higher compared to ash particles at all temperature and relative humidity conditions. Particle characterization analysis shows that surface elemental composition of ash and dust particles was similar; however, the structural properties of ash samples were different.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2010

Feedstock Quality Factor Calibration and Data Model Development

The goal of the feedstock assembly operation is to deliver uniform, quality-assured feedstock materials that will enhance downstream system performance by avoiding problems in the conversion equipment. In order to achieve this goal, there is a need for rapid screening tools and methodologies for assessing the thermochemical quality characteristics of biomass feedstock through the assembly process. Laser-induced breakdown spectroscopy (LIBS) has been identified as potential technique that could allow rapid elemental analyses of the inorganic content of biomass feedstocks; and consequently, would complement the carbohydrate data provided by near-infrared spectrometry (NIRS). These constituents, including Si, K, Ca, Na, S, P, Cl, Mg, Fe and Al, create a number of downstream problems in thermochemical processes. In particular, they reduce the energy content of the feedstock, influence reaction pathways, contribute to fouling and corrosion within systems, poison catalysts, and impact waste streams.

09 BIOMASS FUELS↗
DOE OSTI2019

Structure and Properties of Epoxy/Fly Ash System: Influence of Filler Content and Surface Modification

Epoxy resin composites filled with pristine and organomodified fly ash were prepared and examined. The fly ash used is CaO-rich due to the origin of lignite from the northern Greece area and the power plants in Kozani. As matrix, the epoxy system with curing agent triethylenetetramine was used. A combination of mechanical stirring and ultrasonication was used for highly dispersed fly ash composites. SEM, FTIR spectroscopy and XRD measurements were used to study dispersion homogeneity, structure, degree of aggregation/agglomeration and interface formation of the matrix with the fly ash particles. The properties E′, E″ and relaxations α-(T{sub g}) and β-(Τ{sub β}) of the composites were assessed by DMA. Also, DSC and TGA measurements were used to characterize the thermal properties. Interesting results concerning the effect of the surface organomodification of fly ash on the network formation and the thermomechanical properties of the composites were derived. XRD and FTIR measurements reveal that the functional groups present on the surface of fly ash particles play a dominated role to interface formation. DMA results show that the fly ash surface modification affects the thermodynamic properties of the composites. Additionally, there is evidence showing that the short-scale β-relaxation is also affected by the fly ash surface organomodification.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Electromagnetic wave absorption of multifunctional cementitious composites incorporating polyvinyl alcohol (PVA) fibers and fly ash: Effects of microstructure and hydration

Highlights: • The cementitious composite shows excellent wide-band electromagnetic wave absorption in a frequency range of 2–18 GHz. • The PVA fibers and the fly ash change the dielectric properties of the cementitious composite by Debye polarization. • The iron oxide of the cementitious binders contributes to the magnetic properties of the composites. • The impacts of the microstructure and the hydration of the cementitious composite on its microwave absorption are analyzed. This paper devises a novel method for the adjustment of the pore structure and the hydration of cement to improve the electromagnetic wave absorption of the cementitious composites incorporating polyvinyl alcohol (PVA) fibers and fly ash in a frequency range of 2–18 GHz. The underlying mechanism of the absorption is investigated to explore the possibility of the structural and functional integration of these composites. The electromagnetic parameters of the prepared cementitious composites and those of the raw materials are analyzed in a frequency range of 0.5–18 GHz. Moreover, the pore structure and the chemical environment of the cementitious composites are examined by mercury intrusion porosimetry (MIP), back-scattered electron detector (BSE), and X-ray photoelectron spectroscopy (XPS). The results indicate that the PVA fibers and the high-volume fly ash have a positive effect on electromagnetic wave absorption of the cementitious composites through the adjustment of their pore structure and hydration.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Ranking Coal Ash Materials for Their Potential to Leach Arsenic and Selenium: Relative Importance of Ash Chemistry and Site Biogeochemistry

The chemical composition of coal ash is highly heterogeneous and dependent on the origin of the source coal, combustion parameters, and type and configuration of air pollution control devices. This heterogeneity results in uncertainty in the evaluation of leaching potential of contaminants from coal ash. The goal of this work was to identify whether a single leaching protocol could roughly group high-leaching potential coal ash from low-leaching potential coal ash, with respect to arsenic (As) and selenium (Se). We used four different leaching tests, including the Toxicity Characteristic Leaching Protocol (TCLP), natural pH, aerobic sediment microcosms, and anaerobic sediment microcosms on 10 different coal ash materials, including fly ash, lime-treated ash, and flue gas desulfurization materials. Leaching tests showed promise in categorizing high and low-leaching potential ash materials, indicating that a single point test could act as a first screening measure to identify high-risk ash materials. However, the amount of contaminant leached varied widely across tests, reflecting the importance of ambient conditions (pH, redox state) on leaching. These results demonstrate that on-site geochemical conditions play a critical role in As and Se mobilization from coal ash, underscoring the need to develop a situation-based risk assessment framework for contamination by coal ash pollutants.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Reactive transport modeling and characterization of concrete materials with fly ash replacement under carbonation attack - 15477

There currently lacks sufficient knowledge to accurately characterize structural, hydraulic, and chemical performance of cementitious materials that are required to contain and shield nuclear waste for thousands of years. There are a number of degradation methods that can affect the integrity of these materials over this time frame including carbonation which lowers the alkalinity of the material and can induce cracking in materials with steel reinforcement. The rate and extent of carbonation in these materials is impacted by the addition of fly ash and its composition which can vary depending on the fly ash source. To characterize the carbonation reaction, the changes in the microstructure and elemental distribution as a function of extent of carbonation and fly ash type were evaluated using scanning electron microscopy (SEM) coupled with energy dispersive x-ray spectroscopy (EDS). Micro-concretes were prepared with no fly ash (control case) and with fly ash of various calcium compositions. The progression of the carbonation front was observed in the backscattered electron images by the formation of calcium carbonate and depth was confirmed with a phenolphthalein pH indicator test. The migration and deposition of chemical species were observed in carbonated regions from EDS data and were explained based on the changes in material alkalinity and solubility determined from EPA Method 1313 (Liquid-solid partitioning (LSP) as a function of eluate pH). The changes in mass transport properties from carbonation were observed using EPA Method 1315 (Mass transfer rates in monolithic and compacted granular materials using semi-dynamic tank leaching procedures). The carbonation reaction in each material was simulated using LeachXS/ORCHESTRA, a reactive transport modeling tool, which provided further evidence of localized deposition and migration of chemical species due to changes in speciation and solubility. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Corrosion and Chemical Characterization of Bio-Oils from Biomass with Varying Ash and Moisture Contents

As part of the Feedstock Conversion Interface Consortium four samples of pine chips (all combinations of low and high moisture and ash content) were collected and processed for fast pyrolysis. The prepared biomass samples were liquefied at the National Renewable Energy Laboratory (NREL) using the fast pyrolysis process. Following some characterization of the bio-oils at NREL, the bio-oils were shipped to Oak Ridge National Laboratory (ORNL) for corrosion testing and further characterization.The content and composition of ash in each bio-oil was determined. Corrosion testing consisted of exposing selected metallic and elastomer samples for 1000 hr at 50°C and for longer times at room temperature as well as electrochemical impedance spectroscopy measurements to assess relative corrosivity of the bio-oils. Chemical characterization was conducted to identify the corrosive component of the bio-oils as well as to define the chemical differences among the oils. It was hypothesized that there could be a catalytic effect from the higher ash content in two of the biomass sources. Results of these characterization and corrosion studies will be reported.

Keiser, Jim↗