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DOE OSTI2021

Land management effects on wet aggregate stability and carbon content

Land management affects soil structure and many other soil properties and processes. Our objectives were to evaluate soil organic C (SOC), aggregate size distribution, aggregate-associated C, and soil structure as affected by long-term land management and slope. A chronosequence of 38 on-farm sites with low to high (5–18%) slopes was selected to evaluate 5–40 yr of management. The sites were classified as business as usual (BAU) cropland (BAU-Crop), BAU pasture (BAU-Past), newly established conservation reserve program (CRP) areas (CRP-New), and established CRP (CRP-Old). Soil samples were collected from the 0-to-5- and 5-to-15-cm depth increments and processed for soil property measurements including fractionation by wet sieving into five aggregate size classes (>2,000, 1,000–2,000, 500–1,000, 250–500, and 53–250 μm). Within the surface 5 cm, mean weight diameter (MWD) and geometric mean diameter (GMD) were used to characterize soil structural stability. The BAU-Past and CRP-Old sites had 79% more macroaggregates (>2,000, 1,000–2,000, and 500–1,000 μm), 123% higher MWD, 38% higher GMD, and 47% higher SOC than BAU-Crop or CRP-New sites. The 5-to-15-cm depth increment showed a similar but lower magnitude response. Aggregate-associated C was quantified using a constant soil mass that reflected aggregate size distribution to prevent overestimating C content. Lower-slope locations had more SOC, more macroaggregates, more C associated with macroaggregates, and higher GMD and MWD compared with high-slope locations across all management classifications and soil depths. The results support our hypothesis that the high-slop soils may benefits from specific management decisions than the lower-sloping soils as a function of landscape property. We recommend reestablishing grassland on sloping land that is susceptible to excessive soil erosion, although those practices will likely take a long time to restore soil structural stability and SOC content to precultivation levels.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2021

Root water uptake of biofuel crops revealed by coupled electrical resistivity and soil water content measurements

Abstract Biofuel crops, including annuals such as maize ( Zea mays L.), soybean [ Glycine max (L.) Merr.], and canola ( Brassica napus L.), as well as high‐biomass perennial grasses such as miscanthus ( Miscanthus × giganteus J.M. Greef & Deuter ex Hodkinson & Renvoiz), are candidates for sustainable alternative energy sources. However, large‐scale conversion of croplands to perennial biofuel crops could have substantial impacts on regional water, nutrient, and C cycles due to the longer growing seasons and differences in rooting systems compared with most annual crops. However, due to the limited tools available to nondestructively study the spatiotemporal patterns of root water uptake in situ at field scales, these differences in crop water use are not well known. Geophysical imaging tools such as electrical resistivity (ER) reveal changes in water content in the soil profile. In this study, we demonstrate the use of a novel coupled hydrogeophysical approach with both time domain reflectometry soil water content and ER measurements to compare root water uptake and soil properties of an annual crop rotation with the perennial grass miscanthus, across three growing seasons (2009–2011) in southwest Michigan, USA. We estimated maximum root depths to be between 1.2 and 2.2 m, with the vertical distribution of roots being notably deeper in 2009 relative to 2010 and 2011, likely due to the drought conditions during that first year. Modeled cumulative ET of both crops was underestimated (2–34%) relative to estimates obtained from soil water drawdown in prior studies but was found to be greater in the perennial grass than the annual crops, despite shallower modeled rooting depths in 2010 and 2011.

Kuhl, Alexandria S.↗

DOE OSTI2017

Total Fatty Acid Content Determination of Whole Microalgal Biomass Using In Situ Transesterification

The aliphatic chains of fatty acids are the most prominent and potentially the highest value precursor constituents of algal biomass, and thus accurately quantifying the algal biomass total fatty acid content is a prerequisite for comparing algal strains, growth conditions, and processes. Direct, acid-catalyzed transesterification of whole microalgal biomass is a simple, effective, and widely used method to determine the fatty acid content in whole algal biomass. Such a direct transesterification procedure typically covers the following steps: first, solubilizing the lipids in the biomass matrix and then liberating the fatty acids to make these available for catalytic upgrading to fatty acid methyl esters (FAMEs), subsequent extraction into hexane, and then quantification by gas chromatography. The method we describe here requires less than 10 mg of biomass per sample and is considered high-throughput and highly accurate.

09 BIOMASS FUELS↗

DOE OSTI2018

Total Protein Content Determination of Microalgal Biomass by Elemental Nitrogen Analysis and a Dedicated Nitrogen-to-Protein Conversion Factor

Accurately determining protein content is important in the valorization of algal biomass in food, feed, and fuel markets, where these values are used for component balance calculations. Conversion of elemental nitrogen to protein is a well-accepted and widely practiced method, but depends on developing an applicable nitrogen-to-protein conversion factor. The methodology reported here covers the quantitative assessment of the total nitrogen content of algal biomass and a description of the methodology that underpins the accurate de novo calculation of a dedicated nitrogen-to-protein conversion factor.

09 BIOMASS FUELS↗

DOE OSTI2019

Analysis of Abdominal Radiology fellowship website content and comprehensiveness

Purpose: Fellowship programs’ online content plays a key role in prospective Abdominal Radiology applicants’ evaluation of programs. The purpose of this study is to examine the online accessibility of Abdominal Radiology fellowships, the comprehensiveness of the program websites’ content, and evaluate whether specific program characteristics are associated with differentiated website comprehensiveness. Methods: A list of 67 Abdominal Radiology fellowship programs was obtained from the Society of Abdominal Radiology (SAR) website. Each of the 65 publicly-available fellowship websites was scored for the presence of 19 binary variables related to the program’s attributes and curriculum to assess informational comprehensiveness. Comprehensiveness scores were compared by program characteristics (accreditation status, region, and size) using Kruskal–Wallis and two-tailed t tests. Results: Mean comprehensiveness score of Abdominal Radiology fellowship websites as measured by online criteria met was 52.6% (10.0 ± 3.0/19). Application requirements and information, rotation scheduling, and program director contact were found on more than 87.5% of the 65 websites, whereas salary and benefits, social information, and alumni were listed on fewer than 33.8% (22/65) of websites. Program accreditation status, region, and size were not associated with difference in mean comprehensiveness scores. Conclusions: There is a discrepancy between information commonly sought by prospective Abdominal Radiology fellowship applicants and what is available on fellowship program websites. Programs and applicants alike may benefit from programs strengthening their online material.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2017

Characterization and enzymatic hydrolysis of wood from transgenic Pinus taeda engineered with syringyl lignin or reduced lignin content

Softwood is an abundant resource; however, currently its utilization for bioconversion to obtain platform sugars is limited. Pinus taeda trees which were genetically modified to either produce S lignin or to decrease lignin content were characterized with a suite of analytic techniques. Syringyl lignin was visualized in the secondary xylem of one genetic line with Maule staining. Solid-state nuclear magnetic resonance identified the S lignin units were coupled into the lignin through β-O-4 linkages, and thioacidolysis measured approximately 13% S lignin content in the same sample. Reductions of the lignin of as much as 33% were observed in the transgenics. To better understand how these modifications affect bioconversion, their amenability to hot water and dilute acid pretreatments and enzymatic hydrolysis was evaluated. Lignin reductions resulted in 1.9-3.2-fold increases in glucose release compared to the control. However, no apparent benefit was observed by S lignin incorporation at the concentrations reported in this study. Finally, these results highlight the potential for softwood cell wall properties to be improved for bioenergy/biochemical applications.

09 BIOMASS FUELS↗

DOE OSTI2021

Direct determination of cellulosic glucan content in starch-containing samples

A simple and highly selective analytical procedure is presented for the determination of cellulosic glucan content in samples that contain both cellulose and starch. This method eliminates the unacceptably large compounding errors of current two-measurement methods. If both starch and cellulose are present before analytical hydrolysis, both will be hydrolyzed to glucose causing bias and inaccuracy in the method. To prevent this interference, the removal of starch prior to cellulosic quantification is crucial. The method presented here is a concise in-series procedure with minimal measurements, eliminating large compounding errors. Sample preparation consists of a starch extraction employing enzymatic hydrolysis followed by a simple filtration and wash. The samples are then subjected to a two-stage acid hydrolysis. The concentration of glucose is determined by ion exchange high-performance liquid chromatography with a Pb 2+ column and a refractive index detector. The cellulosic glucan content is calculated based on the initial dry weight of the starting material. Data for the native biomass materials studied show excellent reproducibility, with coefficients of variance of 3.0% or less associated with the method. This selectivity for cellulosic glucan by the procedure was validated with several analytical techniques such as liquid chromatography coupled with mass spectrometry (LC–MS), Raman spectroscopy, and nuclear magnetic resonance.

09 BIOMASS FUELS↗

DOE OSTI2018

Role of Ti Content on the Occurrence of the 3309-cm{sup –1} Peak in FTIR Absorption Spectra of Ruby Samples

The study is based on the determination of trace elements in ruby samples, Ti in particular, using laser ablation inductively coupled plasma mass spectrometry (LA–ICP–MS). The samples were then divided into three groups: high (≥ 200 ppma), moderate (100–200 ppma), and low (≤ 50 ppma) Ti content. In addition, X-ray absorption spectroscopy (XAS) was employed to confirm that the Ti oxidation state was Ti{sup 4+}. The heat experiment conditions were set at 800, 1200, and 1650°C to investigate the transformation of the –OH vibration in the FTIR spectra of ruby samples. The FTIR spectra showed that samples containing a low Ti concentration did not show the 3309-cm{sup –1} absorption peak either before or after heating at any of the designed temperatures. An obvious 3309-cm{sup –1} peak appeared only in samples with a moderate to high Ti content after heating at ≥ 1200°C. The results also suggest that, in addition of Ti{sup 4+}, the occurrence of the 3309-cm{sup –1} peak in the FTIR spectra is strongly affected by the charge compensation of –OH in Al sites, i.e., the structural –OH; thus, the structural –Ti–OH stretching in the ruby samples. Hence, for gemological identification, the 3309-cm{sup –1} peak can be applied to indicate whether a ruby has undergone heat treatment if those samples contain enough Ti ions in their structure, i.e., Ti ≥ 100 ppma. This condition is usually found in ruby samples from major deposits such as Mong Hsu and Mogok, Myanmar; Luc Yen, Vietnam; and Montopuez, Mozambique.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Influence of Iron Content on Microstructure and Magnetic Properties of Sr{sub 0.3}La{sub 0.4}Ca{sub 0.3}n(Fe{sub 2}O{sub 3})Co{sub 0.4}

In this work, the hexagonal ferrite Sr{sub 0.3}La{sub 0.4}Ca{sub 0.3}n (Fe{sub 2}O{sub 3})Co{sub 0.4}, where n ranging from 5.5 to 6.0 with a step of 0.1, and magnetic powders and magnets were synthesized by solid-states reaction. The microstructure of the magnetic powders was investigated by X-ray diffraction (XRD). And then we can found that a single magnetoplumbite phase is obtained for magnetic powders as a result when 5.6 ≤ n ≤ 5.8. When the iron content in the magnetic powders increased continuously, the diffraction peaks of α-Fe{sub 2}O{sub 3} were observed. Scanning electron microcopy (SEM) was used to explore the micrographs of the magnets and the hexagonal-shaped crystals were found obviously. The magnetic properties of the M-type hexagonal ferrites Sr{sub 0.3}La{sub 0.4}Ca{sub 0.3}n(Fe{sub 2}O{sub 3})Co{sub 0.4} were studied by using vibrating sample magnetometry. The saturation magnetization (M{sub s}) first increased and then began to decrease with the n increasing. While the coercivity first decreased with the n from 5.5 to 5.9 and then increased when n ≥5.9. The coercivity (H{sub c}) of the hexagonal ferrite Sr{sub 0.3}La{sub 0.4}Ca{sub 0.3}n(Fe{sub 2}O{sub 3})Co{sub 0.4} reaches the maximum value (H{sub c} = 1130 Oe) when the iron content (n = 5.5).

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

Effect of the Ce Content on the Magnetic Properties and Microstructure of CeCo{sub 5}-based Sintered Bulk Magnets

CeCo{sub 5}-based magnets have recently attracted much attention due to their moderate magnetic performance and low cost. Nevertheless, there have been few studies on the effects of Ce content on the magnetic properties and microstructures of CeCo{sub 5}-based magnets. In response to this, the magnetic properties of sintered bulk magnets with nominal compositions of Ce(Co{sub 0.73}Cu{sub 0.135}Fe{sub 0.135}){sub z} (z = 4.95, 5.15, 5.35, and 5.55), prepared by the conventional powder metallurgy method, were investigated here. Based on experimental findings, it was shown that Ce(Co{sub 0.73}Cu{sub 0.135}Fe{sub 0.135}){sub 5.15} sintered bulk magnets had comprehensive magnetic properties—maximum energy product of 80 kJ m{sup − 3} (10 MGOe) and intrinsic coercivity (H{sub cj}) of 452 kA m{sup − 1} (5.69 kOe)—superior to those previously reported by us. For z = 5.35 and 5.55, due to the presence of the minor Ce{sub 2}Co{sub 17} phase (which has a Curie temperature (T{sub c}) < 20 °C), magnets had low H{sub cj} values. Based on x-ray diffraction and scanning electron microscopy observations, it was suggested that the volume fraction of the 1:5 matrix phase was the main factor determining the H{sub cj} of CeCo{sub 5}-based sintered bulk magnets obtained with different Ce contents. Furthermore, the importance of the dispersion characteristics of the Ce{sub 2}O{sub 3} phase within the matrix was emphasized. Uniform dispersion of the Ce{sub 2}O{sub 3} phase can significantly improve the overall magnetic performance of CeCo{sub 5}-based magnets.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

Effects of Iron Contents on the Vortex State in Fe{sub x}Se{sub 0.5}Te{sub 0.5}

We investigate the effects of iron content on the upper critical field (H{sub c2}) and the activation energy U(T) in thermally activated flux flow in Fe{sub x}Se{sub 0.5}Te{sub 0.5} near the superconducting transition temperature T{sub c}. The variations in H{sub c2}(T) with temperature are analyzed using Ginzburg-Landau (GL), Werthamer-Helfand-Hohenberg (WHH) models along with the empirical relation (ER). The obtained values of H{sub c2}(0) depend strongly on the model and the criteria used to determine the transition temperature. However, the general trend is that that H{sub c2}(0) increases with the increasing Fe content. The activation energy U(T) is maximum for x = 1 and rapidly suppressed by excess or deficiency of iron. The low values of U(T) (∼10 meV) reflect the low vortex-pinning nature (due to defects, vacancies, etc.) in the Fe{sub x}Se{sub 0.5}Te{sub 0.5} superconductor.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2016

Influences of superalloy composition and Pt content on the oxidation behavior of gamma–gamma prime NiPtAl bond coatings

Here, the effects of superalloy composition and Pt content on the high-temperature oxidation behavior of γ–γ’ NiPtAl diffusion coatings were investigated over the temperature range of 1050–1150 °C. Simple NiPtAl diffusion coatings with 7 or 12 µm electroplated Pt thickness were evaluated in 1-h cycles in dry O 2 for up to 2500 cycles on four superalloys: directionally solidified (DS) alloy 142, 1st generation single-crystal (SX) alloy 1483, and 2nd generation SX alloys X4 and N5. Coatings on high-Hf alloy 142 experienced severe internal oxidation of Hf at all temperatures. Coatings on ~5 at.% Ti alloy 1483 were protective at 1050 °C, but exhibited severe scale spallation at 1100 °C, with extensive formation of Ti- and Ni-rich oxides at the gas interface. Coatings with 7-µm Pt on X 4 were extremely protective at 1100 °C, but failed rapidly at 1150 °C, which also was associated with the formation of Ti-rich oxides. Increasing the coating Pt content on X 4 improved the 1150 °C oxidation behavior. Coatings on Ti-free N 5 showed the best performance at 1150 °C, especially with 12-µm Pt. Although γ–γ’ coatings can exhibit outstanding cyclic oxidation resistance with minimal Al depletion, they appear to be sensitive to substrate composition, as well as eventual Pt depletion due to interdiffusion.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Effects of Copper Content and Mold Temperature on the Hot Tearing Susceptibility of Mg-7Zn-xCu-0.6Zr Alloys

The effects of copper (Cu) content and mold temperature on the hot tearing susceptibility (HTS) of Mg-7Zn-xCu-0.6Zr (x = 0, 1, 2) alloys were investigated experimentally using a T-type hot tearing mold. The crack volumes were measured by paraffin permeation method, and the solidification process was analyzed by thermal analysis and by using the Clyne and Davies model. The microstructure and morphology of the crack zone of Mg-7Zn-xCu-0.6Zr alloys were characterized by scanning electron microscopy, and the composition of alloys was analyzed by X-ray diffraction. The results showed the formation of a new phase of MgZnCu in the alloys with Cu addition. Moreover, addition of Cu also led to the refinement of microstructures of Mg-7Zn-xCu-0.6Zr alloys. The HTS of Mg-7Zn-xCu-0.6Zr alloys decreased with the increase in both the content of Cu and the mold temperature.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Investigation of Effects of SiO{sub 2} Content and Cooling Rate on Crystallization in Fe{sub 2}O{sub 3}-CaO-SiO{sub 2} System Using In Situ Confocal Laser Scanning Microscopy

The crystallization behaviors of the Fe{sub 2}O{sub 3}-CaO-SiO{sub 2} system in a non-equilibrium state with various chemical compositions and cooling rates were investigated by confocal laser scanning. Equilibrium samples were prepared in melt states and cooled at a rate of 1 K/min to produce samples in quasi-equilibrium states. The effect of SiO{sub 2} on the phase constitution was investigated using Image Analyzer, and the changes of the phase ratios were analyzed using activity values of Fe{sub 2}O{sub 3} calculated using FactSage 7.1. The Continuous cooling transformation diagram of the Fe{sub 2}O{sub 3}-CaO-SiO{sub 2} system was obtained for various cooling rates. The temperatures at which the primary phase formed for various SiO{sub 2} contents and cooling rates differed from the equilibrium temperatures, and the phase-formation temperature ranges varied with the cooling rate. In addition, the reduction degree of each sample was measured to determine the effect of SiO{sub 2} content and cooling rate on the Fe{sub 2}O{sub 3}-CaO-SiO{sub 2} system. The reduction degree in the FeO{sub 3}-CaO-SiO{sub 2} system is dominantly influenced by the SiO{sub 2} bond-phase morphology (CF, C{sub 2}S, C{sub 3}S, or glass) rather than the cooling rate.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Effect of Zr Content on Mechanical Properties of Diamond/Cu-Zr Composites Produced by Gas Pressure Infiltration

Diamond particle-reinforced Zr-alloyed Cu matrix (diamond/Cu-xZr) composites were produced by a gas pressure infiltration route, with x = 0.0, 0.3, 0.5, 0.75, and 1.0 wt.%. The x-ray diffraction, scanning electron microscopy, and transmission electron microscopy characterization confirms the formation of ZrC at the diamond/Cu interface. With increasing Zr content, the tensile, bending, and compressive strengths of the diamond/Cu-Zr composites are found to firstly increase and then decrease. The maximum tensile, bending, and compressive strengths at 0.75 wt.% Zr are 108, 360, and 441 MPa, respectively. The variation of the mechanical properties is attributed to the formation of interfacial ZrC. The increase in amount of ZrC strengthens the interface, but large ZrC particles formed at high Zr content are harmful to the interfacial bonding. The result suggests that the mechanical properties of diamond/Cu composites can be enhanced by Cu matrix alloying with Zr.

36 MATERIALS SCIENCE↗

DOE OSTI2018

The Mechanical and Microstructural Changes of Sn-Ag-Bi Solders with Cooling Rate and Bi Content Variations

The purpose of this study is to investigate the influence of cooling rate and Bi addition on the microstructure evolution and mechanical properties of Sn-3.5Ag alloy. A series of Sn-3.5Ag-xBi solders has been fabricated with Bi content in the range of 0.5-3.5 wt.%. After solution heat treatment at 170 °C for 24 h and subsequent aging heat treatment at 100 °C for 2 h, samples were divided into two groups. One group was rapidly quenched into iced water (water quenching) for the fast cooling rate (20 °C/s), while the second group was slowly cooled (furnace cooling) in the furnace for the slow cooling rate (0.2 °C/s) after the furnace reflow. The microstructural evolutions of the present solders have been investigated using x-ray diffraction and scanning electron microscopy. The microhardness was measured to correlate the mechanical properties to alloy compositions and cooling rate. It was found that the microhardness of Sn-3.5Ag-xBi solders increased with increasing cooling rate. The indentation creep curves have been evaluated from the obtained microhardness values. Results revealed the steady-state creep rate decreased with increasing Bi content exhibiting an anomalous behavior at 2.5Bi. The reason for improved creep resistance of Sn-3.5Ag-xBi solders is the result of the combination of the solid solution strengthening and precipitation strengthening of Bi. The mean values of stress exponent indicated that the operative creep mechanism is dislocation climb.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Effect of Ni Content on Double-Target Co-sputtered CrNiN Coatings

Double-target co-sputtered CrNiN coatings were deposited by DC-pulsed magnetron reactive sputtering. The nickel content increases from 0.7 to 5.0 at.% with the increased Ni target current from 0.10 to 0.40 A. The influence of Ni content on preferred orientation and properties of CrNiN coatings was investigated. The results show that the doped Ni enters CrN to form (Cr,Ni)N solid solution. CrNiN coatings are mainly composed of CrN phase and demonstrate CrN(111) preferred orientation. All the coatings present columnar growth pattern. And the less obvious the preferred orientation, the more intense competitive growth, the less sufficient the columnar growth, the finer the columnar crystal and the denser the microstructure. In spite of the most dense structure with finest grains, the hardness of CrNiN coating containing 0.7 at.% Ni is the lowest. The hardness is affected by multiple effects of preferred orientation, grain size, solid solution strengthening, morphology and stress, especially the intensity degree of preferred orientation.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Microstructure and Three-Point Bending Fatigue Behavior of Al-Cu-Mg-Ag Alloys with Various Mg Contents

This paper presents an investigation on the influence of Mg content on the microstructures, tensile properties and three-point bending fatigue behavior of Al-Cu-Mg-Ag alloys. The results indicate that the alloy containing 0.70 wt.% Mg possesses lower tensile properties and higher fatigue performance compared to the one with 1.15 wt.% Mg. Increasing Mg content in Al-Cu-Mg-Ag alloys can enhance the nucleation and precipitation of Ω phase, as well as increase the volume fraction and number density of constituent particles. The investigation of the fatigue crack initiation and growth behavior of Al-Cu-Mg-Ag alloy using interrupted fatigue tests suggests that micro-cracks mainly nucleate on Al{sub 2}Cu constituent particles and the fatigue life is mainly associated with the density of constituent particles.

36 MATERIALS SCIENCE↗