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At least 37 records · Page 2

An NDE Approach for Characterizing Quality Problems in Polymer Matrix Composites

Polymer matrix composite (PMC) materials are periodically identified appearing optically uniform but containing a higher than normal level of global nonuniformity as indicated from preliminary ultrasonic scanning. One such panel was thoroughly examined by nondestructive (NDE) and destructive methods to quantitatively characterize the nonuniformity. The NDE analysis of the panel was complicated by the fact that the panel was not uniformly thick. Mapping of ultrasonic velocity across a region of the panel in conjunction with an error analysis was necessary to (1) characterize properly the porosity gradient that was discovered during destructive analyses and (2) account for the thickness variation effects. Based on this study, a plan for future NDE characterization of PMC's is presented to the PMC community.

Roth, Don J.↗

Prediction and Verification of Ductile Crack Growth from Simulated Defects in Strength Overmatched Butt Welds

Defects that develop in welds during the fabrication process are frequently manifested as embedded flaws from lack of fusion or lack of penetration. Fracture analyses of welded structures must be able to assess the effect of such defects on the structural integrity of weldments; however, the transferability of R-curves measured in laboratory specimens to defective structural welds has not been fully examined. In the current study, the fracture behavior of an overmatched butt weld containing a simulated buried, lack-of-penetration defect is studied. A specimen designed to simulate pressure vessel butt welds is considered; namely, a center crack panel specimen, of 1.25 inch by 1.25 inch cross section, loaded in tension. The stress-relieved double-V weld has a yield strength 50% higher than that of the plate material, and displays upper shelf fracture behavior at room temperature. Specimens are precracked, loaded monotonically while load-CMOD measurements are made, then stopped and heat tinted to mark the extent of ductile crack growth. These measurements are compared to predictions made using finite element analysis of the specimens using the fracture mechanics code Warp3D, which models void growth using the Gurson-Tvergaard dilitant plasticity formulation within fixed sized computational cells ahead of the crack front. Calibrating data for the finite element analyses, namely cell size and initial material porosities are obtained by matching computational predictions to experimental results from tests of welded compact tension specimens. The R-curves measured in compact tension specimens are compared to those obtained from multi-specimen weld tests, and conclusions as to the transferability of R-curves is discussed.

Nishioka, Owen S.↗

Impact of sub-core scale heterogeneity on CO2/brine multiphase flow for geological carbon storage in the Minnelusa sandstone

CO2 geological storage in deep saline aquifers is a mitigation option for CO2 emissions due to its large storage capacity and immediate accessibility. Accurately determining the CO2-brine relative permeability curves is key to the evaluation of CO2 injectivity and sweep efficiency in reservoir simulation as well as the CO2 injection in the field. This study highlights the remarkable effects of sub-core scale heterogeneity on the CO2-brine multiphase flow properties of the Minnelusa Sandstone in Wyoming. Two unsteady state CO2-brine drainage experiments were performed on the two samples. The first sample exhibits slanted laminated structure, while the second one represents a more homogeneous sandstone system. The CO2 saturation distributions during drainage reveals that the main variation in multiphase flow properties of two core samples were attributed to the porosity distribution that leads to the capillary pressure heterogeneity. Assisted history matching was used to obtain the respective relative permeability curves, which suggests heterogeneity-dependent behavior. In addition, sensitive and uncertainty analyses indicate that physical and petro-physical properties of low-porosity and low-permeability bedding layers exert marked effects on CO2 front breakthrough time and brine production. The results presented in this study help to gain insight into the CO2-brine multiphase flow properties in heterogeneous sandstones and can pave the way for the upscaling of CO2 migration and field-scale simulation accurately. This work is funded under the Department of Energy CarbonSAFE program (awards DE-FE0031624 DE0031891).

Kou, Zuhao↗

An Exploratory Study of the Microstructure of Mullite Fibers

The microstructures of mullite composition fibers were examined by transmission electron microscopic techniques and by X-ray diffraction analyses. Both spun and monofilament fiber structures contained little porosity, nor did the degree of porosity change after heating the monofilament to 1205 C for one half hour. Thermal exposure produced crystallite growth and nucleation from the amorphous phase in all three of the spun fibers. After 116 hours at 1426 C, the crystallites of the standard spun fibers became contiguous. In addition, the surface crystallites of these fibers were found to be more than twice as large as the interior crystallites.

Santoro, G.↗

Factors controlling pore network development of thermally mature Early Palaeozoic mudstones from the Baltic Basin (N Poland)

Understanding the formation of pore space, especially in low porosity shales (as source rocks and as unconventional resources), is critical to the oil and gas industry, since pores control the space available for hydrocarbon and participate in hydrocarbon transport. We examined 87 Ordovician and Silurian mudstone samples collected from four wells located in the Pomeranian part of the Baltic Basin (northern Poland), one of the primary Polish targets for hydrocarbon exploration. These samples represent the Pelplin, the Paslek, the Jantar, the Prabuty, and the Sasino Formations, which still requires more detailed porosity studies. Our study aimed to identify factors controlling porosity development, by applying bulk techniques (organic petrology and TOC analyses, quantitative mineralogy, and porosimetry) as well as nano- to microscale techniques (thin section petrography, electron microscopy). The studied samples are mainly argillaceous mudstones. The results of porosimetry measurements, combined with image analysis, indicate that the pores of all studied rocks are dominated by micropores (pores < 2 nm in diameter), mesopores (2-50 nm in diameter) and small macropores. The SEM images showed three main pore types: a) voids related to clay mineral aggregates, b) pores inside organic matter particles, and c) pores between other mineral grains. In the Jantar and Sasino mudstones, the organic matter content and its thermal maturity control porosity. The occurrence of solid bitumen in the rocks from these formations reduces samples’ mesoporosity because of the pore-clogging effect. In contrast, in the Paslek and Prabuty Formations, there is low organic matter content and specific surface area and the volume of mesopores increase with clay minerals content. In the Pelplin mudstones, there are no prevailing factors controlling porosity. As a result, we suggest that a combination of SEM image analysis and dual liquid porosity (DLP) measurements is a powerful method to assess porosity available for petroleum flow in mudstones.

03 NATURAL GAS↗

Coordinated analyses of hydrated Kuiper Belt dust

We report on coordinated mineralogical, chemical, and isotopic analyses of hydrated carbon-rich interplanetary dust particles (IDPs). We focus on hydrated IDPs that contain high solar flare track densities consistent with an origin in outer Solar System bodies such as Edgeworth-Kuiper belt objects (EKBOs) [1]. We are searching for evidence of the heavy water reservoir predicted by self-shielding models [2]. The IDPs were embedded in sulfur and microtome thin sections were obtained for Fourier-transform infrared (FTIR), transmission electron microscopy (TEM), and nanoSIMS analyses. The IDPs were only partly microtomed and the remainder was extracted from the sulfur and pressed into In or Au for high precision O isotopic analyses. The hydrated IDPs in this study are compact low-porosity objects with a mineralogy dominated by fine-grained saponite and lesser serpentine, Fe-Ni sulfides, Mg-Fe carbonates, rare crystaline silicates, and abundant organic matter. The C in the IDPs is abundant (typically >4X CI) and occurs as isolated nanoglobules and finely disseminated within the phyllosilicate matrix of the IDPs. TEM analyses of the nanoglobules show O-rich, S-depleted rims with higher carbonyl functionality than their cores. FTIR spectra show strong aliphatic C-H stretches consistent with the presence of short-chain aliphatic hydrocarbons in these IDPs. The oxygen isotopic compositions measured in 6 IDPs all plot within error of the CCAM line [3]. For several of the IDPs we were able to obtain multiple analyses. The ∆^(17)O values range from -23‰ up to +3.4‰ with most analyses clustering above the terrestrial fractionation line. The O isotopic compositions and the high C contents of these IDPs are distinct from known hydrated carbonaceous chondrites. The track-rich hydrated IDPs record parent body aqueous alteration effects through interactions with 16O-poor H2O on a EKBO parent body. The aqueous alteration activity likely resulted from the heat generated by collisional processes among EKBOs given that these objects are believed to have accreted late after the decay of 26Al [4].

Lindsay P. Keller↗

Highly Crystalline and Porous Borocarbonitrides as Metal‐Free Catalysts for Boosted N‐Heterocycle Dehydrogenation

Safe and efficient hydrogen storage is pivotal for enabling a clean hydrogen economy. Liquid organic hydrogen carriers (LOHCs) offer a practical solution, but their deployment is hindered by the lack of highly active and economical dehydrogenation catalysts. In this work, we report a metal‐free catalyst design that overcomes the long‐standing trade‐off between crystallinity and surface area in two‐dimensional frameworks for highly efficient dehydrogenation of LOHCs. A flux‐assisted reconstruction strategy transforms amorphous borocarbonitrides (AM‐BCN) into highly crystalline, defect‐rich BCN nanosheets (C‐BCN) with large surface area and accessible porosity, as confirmed by complementary spectroscopic, x‐ray, and neutron analyses. C‐BCN catalyzes the acceptor‐less dehydrogenation of aza‐fused LOHCs with quantitative hydrogen release under mild conditions, outperforming AM‐BCN and previously reported metal‐free scaffolds. Mechanistic insights from x‐ray, neutron scattering, and theoretical calculations identify open C‐B‐N and N‐B‐N defect motifs as the primary active sites. This work establishes a generalizable strategy to engineer crystalline, porous, defect‐rich two‐dimensional lattices and demonstrates a highly active metal‐free platform for LOHC dehydrogenation with high‐purity H 2 generation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Venus: Global radar properties in a geological context

The radar altimetry, roughness (RMS slopes), and reflectivity data acquired for Venus represent the only global radar information available for any of the planets. In addition, the Pioneer Venus radar instrument was able to sound the surface at normal incidence so that it was possible to accurately measure the small-scale surface slopes and reflectivity (dielectric and porosity properties) at the same time as the surface elevation. Analyses of the topography of Venus demonstrate that it differs in its distribution from the Moon, Mars, or the Earth. While the range of topography extends from -2.5 km below the reference level to 11.5 km above, most of Venus falls within 1 km of the mean elevation, this is in sharp contrast to the Earth. The narrow, unimodal nature of the distribution of topography on Venus evidently exerts control on the other radar-derived properties of the surface. When clustering analysis techniques are applied to the Venus radar data sets, the result demonstrates that topographic zones serve as the best criteria for distinguishing regions on Venus which have related radar properties. The individual radar data sets are investigated separately and in conjunction with topography.

Garvin, J. B.↗

Application of Ibuprofen Sodium Dihydrate for Thermochemical Energy Storage

Thermochemical energy storage (TCES) offers a transformative approach to address grid instability by harnessing reversible chemical reactions for efficient heat storage and release. Here, we introduce pharmaceutical organic salt hydrates as a class of materials with exceptional performance for low-grade waste heat recovery. We demonstrate ibuprofen sodium dihydrate (ISD) as an example organic hydrate exhibiting a dehydration temperature range of 60-110 °C and a remarkable dehydration enthalpy of up to 59.5 kJ/mol of water, ideally suited for capturing industrial and residential waste heat. Using rigorous multimodal characterization, including thermogravimetric analysis, differential scanning calorimetry, in-situ FTIR, in-situ PXRD, and NMR, we demonstrate ISD's superior thermal, chemical, and structural stability over 150 hydration-dehydration cycles, achieving an unprecedented cycling efficiency of ~99.9%. Compared to conventional inorganic salt hydrates like strontium chloride hexahydrate and calcium oxalate monohydrate, ISD showcases enhanced durability without deliquescence or pulverization, even under high-humidity conditions. In-situ analyses confirm the transition from ISD to ibuprofen sodium anhydrous (ISA) proceeds with structural reorganization, thereby combining the dehydration mechanism with phase transitions, resulting in higher energy storage capacity. Microstructural analyses reveal that repeated water intercalation and structural transitions aid in creating significant porosity that enhances water transport kinetics, further improving the hydration/dehydration performance. By combining the phase change and chemical dehydration mechanisms, ISD paves the way for designing a new class of organic salt hydrates, offering tunable properties to meet diverse thermal energy storage demands and supporting sustainable grid resilience.

Thangaraj, Kavin C.↗

A cause of the non-solderability of ceramic capacitor terminations

The results of an analysis into the cause of the non-solderability of multiple defective part lots from two capacitor manufacturers are described. This analysis consisted of visual, scanning electron microscopic, surface, and metalographic examinations and analyses. The results indicated that non-solderability results from areas of excess porosity in the termination which are caused by segregation of ink constituents during manufacturing. This segregation can be minimized by proper monitoring and control of process variables; where excess porosity does occur, solderability can be improved by proper precleaning of parts.

Cozzolino, M. J.↗

Distinguishing Indigenous from Contaminating Microorganisms in Rock Samples from a Deep Au Mine in South Africa

The concentration and distribution of microbial biomass within deep subsurface rock strata is not well known To date, most analyses are from water samples and a few cores. Hand samples, block samples and cores from an actively mined Carbon Leader ore zone at 3.2 kilometers depth were collected for microbial analyses. The Carbon Leader was comprised of quartz, S-bearing aromatic hydrocarbons, Fe(III) oxyhydroxides, sulfides, uraninite, Au and minor amounts of sulfate. The porosity of the ore was 1% and the maximum pore throat diameter was less than 0.1 microns; whereas, the porosity of the adjacent quartzite was .02 to .9% with a maximum pore throat diameter of 0.9 microns. Rhodamine dye, fluorescent microspheres, microbial enrichments, autoradiography, phospholipid fatty acid (PLEA) and 16S rDNA analyses were performed on these rock samples and the mining water. The date indicate that the levels of solute contamination less than 0.01% for pared rock samples. Despite this low level of contamination, PLEA, microbial enrichment, DNA and tracer analyses and calculations indicate that most of the viable microorganisms in the Carbon Leader represent gram negative aerobic heterotrophs and ammonia oxidizers that are phylogenetically identical or closely related to service water microorganisms. These microbial contaminants probably infiltrated the low permeability rock through mining-induced microfractures. Geochemical data also detected drilling water in a fault zone approx. 1 meter behind the rock face encountered during coring. The mining induced macrofractures that are common at these great depths act as pathways for the drilling water borne microorganisms into the lower temperature zone that extends several meters into rock strata from the rock face. Combined PLEA and T- RFLP analyses of the service water and Carbon Leader samples indicate that the concentration of indigenous microorganisms was less than 10(exp 2) cells/gram. Such a low concentrations result from the submicron pore throat diameters. PLFA. SO4-35 autoradiography and tracer analyses indicate that the bounding quartzite contains thermophilic sulfate reducing bacteria at 10(exp 3) cells/gram that are not attributable to drilling water contamination. The microorganisms may be surviving on sulfate generated by oxidation of sulfide by radiolytic reactions resulting from the high U concentration in the ore zone. The presence of up to 8,000 ppm of Fe(III) oxyhydroxides in the host rock will also act to recycle sulfide generated by the sulfate reducing bacteria into sulfate. The activity of these sulfate-reducing bacteria may be enhanced by mining induced fracturing which can propagate up to 40 meters into virgin rock where the temperatures are ca. 50 C, and decrepitate of sulfate rich fluid inclusions. In ultra deep mines, judicious application of tracers and multiple microbial characterization techniques can distinguish microbial contamination caused by the near field fracturing and drilling water migration from the indigenous microbial communities in rock strata. The importance of far field fracturing on indigenous microbial communities, however, remains unknown.

Onstott, T. C.↗

Accurate measurement of porosity size and morphology in aluminium alloy laser welds

Conventional two-dimensional optical microscopy is the most common tool for capturing and quantifying keyhole collapse porosity and other defects formed during the laser welding of aluminium alloys. This approach is of limited utility since only a single longitudinal or transverse metallographic cross-section, comprising only a small fraction of the overall weld volume, can be extracted or analysed at a time. X-ray computed tomography tools, on the other hand, enable three-dimensional visualisation and analysis of porosity and defects to be made across the full weld volume. When comparing these two measurement techniques, two-dimensional microscopy tools significantly underestimated the fraction of defects present within the weld at levels between 50% and 80%. Three-dimensional x-ray computed tomography tools also provide a means for accurately characterising the location, size and morphology of irregularly shaped defects. By categorising the defect shapes using a Zingg's shape analysis, in which the distribution of defect morphologies could be quantified as disk, rod and spherical shapes, a transition in defect morphology moving from stationary beam to oscillating beam welds was detected and quantified.

36 MATERIALS SCIENCE↗

Evolution of Pore Structure and Permeability of Rocks Under Hydrothermal Conditions (Final Report)

The physical and transport properties of porous rocks can be altered by a variety of diagenetic, metamorphic, and tectonic processes, and the changes that result are of critical importance to such industrial applications as resource recovery, carbon dioxide sequestration, and waste isolation in geologic formations. The associated interrelationships between rocks, pore fluids and deformation are also key to understanding many natural processes, including dynamic metamorphism, fault mechanics, fault stability and pressure solution creep. In this project, we investigated the changes of permeability and pore geometry owing to inelastic deformation by solution-transfer, brittle fracturing and dislocation creep. In particular, we studied the coupling between pore fluids and deformation in fluid-filled quartz, calcite, mudstones and ultramafic rocks and examine the effects of coupled mechanical and chemical processes on the evolution of porosity and permeability under hydrothermal conditions. The investigations used a combination of techniques, that included triaxial laboratory experiments; uniaxial compressive loading with in situ observations of microstructure; permeability under hydrostatic compression; observations of microstructure using optical and electron microscopes, and micro-CT imaging; and numerical calculations. Laboratory experiments were designed to provide mechanical and transport data under conditions that isolate the particular mechanisms responsible for the changes. The data obtained were used to quantify changes in surface roughness, porosity, pore dimensions and their spatial fluctuations. The results of the experiments and data from image analyses were compared to the results of network, finite-difference and other numerical models to verify the validity of experimentally established relations between permeability and other rock properties. A bibliography for the period from 2015-2019 is appended below. New results obtained in the final year and the unfunded extension period are detailed below.

58 GEOSCIENCES↗

Using block-copolymer nanolithography as a tool to sensitively evaluate variation in chemical dry etching rates of semiconductor materials with sub-5 nm resolution

Ion implantation is a robust and established method to customize the electronic properties of Si. However, fabricating doped, ultrafine semiconductor nanostructures can be challenging. Ion implantation has well-established effects on the dry etch rates of Si, which becomes increasingly consequential as the target dimension shrinks below a few tens of nanometers. While dry etching arrays of block copolymer-templated nanoscale holes (pitch = 37.5 nm, diameter ~25 nm) into p-type, n-type, and undoped Si, we observed that the lateral etch rate was notably larger for the n-type regions than p-type or undoped regions. By doing image analyses on high resolution electron micrographs of the nanostructured hole arrays, we were able to extract the porosity and average radii of the holes with subnanometer sensitivity and compare the relative etch rates between different doping conditions. We found that degenerately doped n-type silicon consistently etches between approximately 17% and 27% faster in the lateral direction than p-type Si, resulting in significantly larger porosity and, consequently, less mechanical stability. Here, we demonstrate that top-down dimensional analysis of a densely packed porous nanostructure is a robust method for assessing extremely small differences in the lateral, chemical etch rate of doped Si to a degree of sensitivity that was previously unachievable. The minute, dense-packed nature of block copolymer self-assembled nanostructures is shown to be ideal for this application. This proposed method could be useful for designing fabrication processes for heterogeneous nanostructures, as slight dry etch rate variations that may be within process tolerance at the micrometer-scale appear to have nontrivial consequences at the nanometer scale.

42 ENGINEERING↗

CFD modeling of turbulent flows around the SSME main injector assembly using porosity formulation

Hot gas turbulent flow distribution around the main injector assembly of the Space Shuttle Main Engine (SSME) and LOX flow distribution through the LOX posts have a great effect on the combustion phenomena inside the main combustion chamber. In order to design a CFD model to be an effective engineering analysis tool with good computational turn-around time (especially for 3-D flow problems) and still maintain good accuracy in describing the flow features, the concept of porosity was employed to describe the effects of blockage and drag force due to the presence of the LOX posts in the turbulent flow field around the main injector assembly of the SSME. Two-dimensional numerical studies were conducted to identify the drag coefficients of the flows, both through tube banks and round the shielded posts, over a wide range of Reynolds numbers. Empirical, analytical expressions of the drag coefficients as a function of local flow Reynolds number were then deduced. The porosity model was applied to the turbulent flow around the main injector assembly of the SSME, and analyses were performed. The 3-D CFD analysis was divided into three parts: LOX dome, hot gas injector assembly, and hydrogen cavity. The numerical results indicate that the mixture ratio at the downstream of injector face was close to stoichiometric around baffle elements.

Cheng, Gary C.↗

Flow Distribution Around the SSME Main Injector Assembly Using Porosity Formulation

Hot gas turbulent flow distribution around the main injector assembly of the Space Shuttle Main Engine (SSME) and Liquid Oxidizer (LOX) flow distribution through the LOX posts have a great effect on the combustion phenomena inside the main combustion chamber. In order to design a CFD model to be an effective engineering analysis tool with good computational turn-around time (especially for 3-D flow problems) and still maintain good accuracy in describing the flow features, the concept of porosity was employed to describe the effects of blockage and drag force due to the presence of the LOX posts in the turbulent flow field around the main injector assembly of the SSME. 2-D numerical studies were conducted to identify the drag coefficients of the flows both through tube banks and around the shielded posts over a wide range of Reynolds numbers. Empirical, analytical expressions of the drag coefficient as a function of local flow Reynolds number were then deduced. The porosity model was applied to the turbulent flow around the main injector assembly of the SSME, and analyses were performed. The 3-D CFD analysis was divided into three parts, LOX dome, hot gas injector assembly, and hydrogen cavity. The numerical results indicate that the mixture ratio at the downstream of injector face was close to stoichiometric around baffle elements.

Cheng, Gary C.↗

Flow Distribution Around the SSME Main Injector Assembly Using Porosity Formulation

Hot gas turbulent flow distribution around the main injector assembly of the Space Shuttle Main Engine (SSME) and Liquid Oxidizer (LOX) flow distribution through the LOX posts have a great effect on the combustion phenomena inside the main combustion chamber. In order to design a CFD model to be an effective engineering analysis tool with good computational turn- around time (especially for 3-D flow problems) and still maintain good accuracy in describing the flow features, the concept of porosity was employed to describe the effects of blockage and drag force due to the presence of the LOX posts in the turbulent flow field around the main injector assembly of the SSME. 2-D numerical studies were conducted to identify the drag coefficients of the flows both through tube banks and around the shielded posts over a wide range of Reynolds numbers. Empirical, analytical expressions of the drag coefficient as a function of local flow Reynolds number were then deduced. The porosity model was applied to the turbulent flow around the main injector assembly of the SSME, and analyses were performed. The 3-D CFD analysis was divided into three parts, LOX dome, hot gas injector assembly, and hydrogen cavity. The numerical results indicate that the mixture ratio at the downstream of injector face was close to stoichiometric around baffle elements.

Cheng, Gary C.↗

A Novel Technique for Distributed Measuring of Strain in the Vadose Zone

Characterizing water content and pressure changes in the vadose zone is important to understanding a variety of geologic processes, ranging from permeability, to evapotranspiration, and aquifer recharge. Changes in water content, or pressure, cause strain in the solid porous medium of the vadose zone, and it is possible that measuring those strains could be used a characterization tool. The Coherence-length-gated Microwave Photonics Interferometry (CMPI) technique measures strain at high resolution along many intervals defined by pairs of reflectors distributed along an optical fiber. This technique has recently been developed at Clemson University, and it has the spatial, and temporal resolution to characterize the strains that are expected to occur with hydrologic changes in the vadose zone. However, the technique has never been used to measure strain in porous media, so its capabilities remain uncertain. The objective of this thesis is to evaluate the ability of using CMPI to measure strain changes in the vadose zone. The research approach consists of conducting laboratory tests using a column filled with sand that was subjected to changes in water content and pressure. An optical fiber with CMPI reflectors was deployed in a high surface area ribbon and used to measure strain along the axis of the column. The column was made from 8-inch, Schedule 40 PVC pipe (75 cm tall, 20 cm inner diameter) and filled with medium-grained sand (K = 2.5x10-6 m/s, porosity = 0.28, Coefficient of Uniformity = 2, van Genuchten (n = 4.34 and  = 0.00039 m-1), Young’s Modulus = 18 – 47 MPa). Five pressure and four temperature sensors attached to probes inserted into the wall. The optical fiber includes five reflectors spaced 10 cm apart on the inside and outside of the column along the vertical axis. Strain measurements are made between pairs of reflectors. The reflectors are created in 250-micron-diameter acrylate-coated single mode Corning SMF28e+ optical fiber using a femtosecond laser. The optical fiber was laminated between two pieces of polyester film creating a large surface area to transfer strain from the porous media to the optical fiber. The experiments were conducted by filling the column from the bottom or infiltrating water from the top. The water was allowed to equilibrate to room temperature prior to each test in order to limit thermoelastic strain. Five injection tests with a rate of 250 ml/min and three infiltration tests at varying rates were conducted, and the results show patterns of strain and pressure are generally similar. Hydrologic conditions define three zones based on the pressure magnitude and distribution. 1.) Ambient Zone where the pressure heads are quasi-static and the pressure gradient is roughly unity (head gradient of zero). This is the uppermost zone and is characterized by negative pressures. 2.) Transition Zone where the pressures increase from ambient to zero, are changing relatively rapidly and the pressure gradient is relatively steep (pressure head gradients of 2). The Transition zone is 10 to 15 cm thick. 3.) Positive Pressure Zone where the pressure is positive, the rate of change is slower than in the transition zone and the gradient is flatter (pressure head gradient 1.1 to 1.2). This is the lowest zone in the column. Injection of water causes the pressure to increase and the three zones to move upward. The Transition zone moves at a rate of approximately 0.0002 m/s +/- .00005, according to analyses of pressure profiles. This is the same as the average velocity of the water calculated as volumetric flux/effective porosity =5.4x10-5 m/s/0.28. Strain signals in the range of 10s  were observed with a noise level of generally less than 0.1  (signal to noise ratio of greater than 100) during injection and drainage. The spatial and temporal distributions of strain caused by injection depend on the location of the moving pressure zones. The locations of the different pressure zones were determined from pressure profiles at different times and these data were transferred to strain time series. This showed that strain in the Ambient pressure zone is either unchanged or slightly compressive, whereas strain in Transition zone is tensile and roughly proportional to the pressure change, and strain ranges from tensile to compressive in the Positive Pressure zone. In general, the strain is variable at the top of the Positive Pressure zone, but it appears to be consistently tensile lower in the zone. The spatial distribution of strain causes three distinct stages in the strain times series measured between pairs of CMPI reflectors. The strain is unchanged or slightly compressive during Stage 1, it increases (positive strain is tensile) approximately linearly at a rate of 0.02 to 0.03 μ/s during the Stage 2, and then flattens out in Stage 3. The strain increases again during Stage 4 of the time series. The pressure also changes in stages. It is unchanged during Stage 1 and then increases relatively rapidly at a rate of between 4 and 10 Pa/s during Stage 2 and continues to increase during Stages 3 and 4, but at a rate slightly slower than during Stage 2 (from 2.5 to 3.5 Pa/s). The rates of pressure and strain change are consistent with basic analyses. The rate of pressurization is similar to the calculated velocity of flow in the saturated zone, and this is similar to the measured velocity of the strain increase. The ratio of the pressurization rate and strain rate during Stage 2 (2.5 (Pa/s) /0.03 (μ/s)) is 80 MPa, which is approximately equal to the upper range expected considering the uniaxial compression and the Young’s Modulus of the sand. An interesting effect occurs when the upper surface of the sand becomes saturated. Significant compression (several 10s of ) occurs as the pressure and saturation increase at the upper surface. Compression occurs throughout the column, but the effect is greatest at the top of the column. The rate of compression is fastest slightly before ponding occurs, but it slows markedly and nearly stops when water starts to accumulate at the surface (ponding). This effect reverses when the surface of the sand is drained, resulting in tension throughout the column. The compression caused by this effect can be as large or larger than the tensile strain that accumulated during filling. This effect was unexpected because increasing pressure is normally associated with tensile strain. Nevertheless, this effect was observed consistently in all tests where the pressure changes at the upper surface, including tests where water was injected from below or infiltrated from above. This effect behaves as if the pore pressure at the upper surface of the sand exerts a normal force on the boundary (increasing pore pressure exerts a downward compression on the boundary). The results of these laboratory experiments indicate that CMPI can measure strain caused by fluid pressure changes in the vadose zone with a signal to noise ratio of 100 or more. Injection and drainage cause a strain signal that is complex, but repeatable. The magnitudes of the strain signal are consistent with magnitudes that are expected based on poroelastic calculations using independently measured properties of the sand. These results indicate that the CMPI technique with an optical fiber laminated in a polyester ribbon generates data that represent the strain distribution during hydrologic processes of imbibition and drainage in variably saturated sand. This suggests that distributed strain measurements using CMPI could be a viable approach for evaluating processes in the vadose zone, laying the groundwork for future field implementation.

47 OTHER INSTRUMENTATION↗