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At least 757 records · Page 42

Development of a Platform for High-Resolution Ion Mobility Separations Coupled with Messenger Tagging Infrared Spectroscopy for High-Precision Structural Characterizations

The ability to uniquely identify a compound requires highly precise and orthogonal measurements. Here we describe a newly developed analytical platform that integrates high resolution ion mobility and cryogenic vibrational ion spectroscopy for high-precision structural characterizations. This platform allows for the temporal separation of isomeric/isobaric ions and provides a highly sensitive description of the ion’s adopted geometry in the gas phase. The combination of these orthogonal structural measurements yields precise descriptors that can be used to resolve between and confidently identify highly similar ions. The unique benefits of our instrument, which integrates a structures for lossless ion manipulations ion mobility (SLIM IM) device with messenger tagging infrared spectroscopy, include the ability to perform high-resolution ion mobility separations and to record the IR spectra of all ions simultaneously. The SLIM IM device, with its 13 m separation path length, allows for multipass experiments to be performed for increased resolution as needed. It is integrated with an Agilent qTOF MS where the collision cell was replaced with a cryogenically held (30 K) TW-SLIM module. The cryo-SLIM is operated in a novel manner that allows ions to be streamed through the device and collisionally cooled to a temperature where they can form noncovalently bound N 2 complexes that are maintained as they exit the device and are detected by the TOF mass analyzer. The instrument can be operated in two modes: IMS+IR where the IR spectra for mobility-selected ions can be recorded and IR-only mode where the IR spectra for all mass-resolved ions can be recorded. In IR-only mode, IR spectra (400 cm –1 spectral range) can be recorded in as short as 2 s for high throughput measurements. Further, this work details the construction of the instrument and modes of operation. It provides initial benchmarking of CCS and IR measurements to demonstrate the utility of this instrument for targeted and untargeted approaches.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Comparability of Liquid Chromatography Tandem Mass Spectrometry Analysis of Dissolved Organic Matter across Laboratories

Non-targeted liquid chromatography tandem highresolution mass spectrometry (LC−MS/MS) is increasingly applied for the structure-resolved chemical analysis of dissolved organic matter (DOM). With new developments in MS instrumentation and analysis software, the approach has gained substantial momentum over the past decade. However, achieving high-quality analytical data that is reproducible and comparable across laboratories can be a bottleneck in non-targeted metabolomics and organic matter chemical analysis, especially for data reuse in repository-scale analyses. Understanding the capabilities as well as challenges of comparing LC−MS/MS data from different laboratories is necessary for inferring global trends from public data sets. To illuminate instrumentation factors that drive differences and variability, we used a standardized data analysis pipeline, including classical (CMN) and featurebased molecular networking (FBMN), to analyze data from a ring trial by 24 laboratories on identical sample sets of algal and DOM extracts that were mixed in predefined concentrations and spiked with standards. Our results showed that data sets from similar mass spectrometer types with unified instrument parameters were qualitatively comparable, resolving the same general trends and shared mass spectral features. Interlaboratory comparability was best for high-intensity features, while low-intensity features showed greater detection variability. Our analysis also highlights challenges when comparing data from instruments with different acquisition rates or operating with less standardized methods. Lastly, we provide recommendations for data integration, public data sharing, standardization, and best practices for standardized LC−MS/MS data acquisition, which will be critical for long-term time series and intercomparability of DOM chemical analyses.

DOM↗

Evaluating Limits of Machine Learning-Assisted Raman Spectroscopy in Classification of Biological Samples

Machine learning (ML)-assisted Raman spectroscopy has become a powerful analytical tool for the classification and identification of analytes; however, technical challenges impacting its detection accuracy have not been thoroughly investigated. This study explores experimental factors affecting classification performance. Among the evaluated ML models, ML algorithms show minimal impact on classification accuracy. Instead, experimental factors, including spectral similarity between tested samples and data quality, dominate detection performance. Increases in spectral noise and spectral similarity significantly reduce classification accuracy. In well-controlled samples with low experimental noise, ML-assisted Raman spectroscopy can discriminate lipid mixtures with a composition difference of 1.85 mol %. To assess the effect of biological heterogeneity, we analyzed single-cell Raman spectra from Saccharomyces cerevisiae strains carrying single, double, or triple gene mutations. Intrinsic cell-to-cell variability introduced substantial spectral differences, severely reducing the accuracy of multiclass classification of these genetically similar strains at the single-cell level. Averaging Raman spectra across multiple cells improved classification accuracy by reducing this spectral variability. We also assess the effectiveness of transfer learning across different Raman spectrometers, specifically by applying an ML model trained on one instrument to another Raman spectrometer. Transfer learning can be improved with proper instrument calibration, highlighting the importance of instrument standardization. Overall, our results demonstrate that data quality and spectral similarity are the primary bottlenecks in ML-assisted Raman spectroscopy. Careful attention to sample preparation, data acquisition, measurement conditions, and instrument calibration is critical to achieving robust and reliable classification performance.

Fungi↗

Calibration and Initial Results of Space Radiation Dosimetry Using the iMESA-R

The integrated Miniaturized Electrostatic Analyzer-Reflight (iMESA-R) is a space weather instrument designed to measure plasma density, temperature, and spacecraft charging, along with total ionizing dose and dose rate. A constellation consisting of five nearly identical instruments has been designed and developed to act as science payloads hosted on-board Department of Defense satellites operating in low-Earth orbit. To validate the dosimetry component of the iMESA-R, a radiation test study was performed to calibrate the dosimeter and ascertain the attenuation due to the instrument aluminum housing. An 80 curie Cobalt-60 radioisotope source emitting beta, X-ray, and gamma ray radiation decay products was used to calibrate the dosimeter response as a function of distance and instrument shielding. We present results of the calibration study along with initial on-orbit data presented from the first operational iMESA-R hosted on-board Space Test Program Satellite 5 in a polar Earth orbit. The initial on-orbit data demonstrate the ability to map the radiation environment, particularly the South Atlantic Anomaly and the auroral regions using total ionizing dose rate due to electrons of E > 1.5 MeV and protons of E > 25 MeV.

79 ASTRONOMY AND ASTROPHYSICS↗

Advancing Cross-Disciplinary Understanding of Land-Atmosphere Interactions

The evolution of disciplinary silos and increasingly narrow disciplinary boundaries have together resulted in one-sided approaches to the study of land-atmosphere interactions—a field that requires a bi-directional approach to understand the complex feedbacks and interactions that occur. The integration of surface flux and atmospheric boundary layer measurements is therefore essential to advancing our understanding. The Land-Atmosphere 2021 workshop (held virtually, June 10-11, 2021) involved almost 300 participants from around the world and promoted cross-discipline collaboration by way of talks from invited speakers, moderated discussions, breakout sessions, and a virtual poster session. The workshop focused on five main theme areas: “big picture” overview, instrumentation and remote sensing, modeling, water, and aerosols and clouds. In talks and breakout groups, there were frequent calls for more AmeriFlux sites to be instrumented for boundary layer height measurements, and for the development of some “super sites” where profiling instruments would be deployed. There was further agreement on the need for the standardization of various datasets. There was also a consensus that funding agencies need to be willing to support the sorts of large projects (including associated instrumentation) which can drive interdisciplinary work. Early-career scientists, in particular, expressed enthusiasm for working across disciplinary boundaries but noted that there need to be more financial support and training opportunities so they would be better prepared for interdisciplinary work. Investment in these career development opportunities would enable today's cohort of early-career scientists to advance the frontiers of interdisciplinary work over the next couple of decades.

54 ENVIRONMENTAL SCIENCES↗

Imaging grain microstructure in a model ceramic energy material with optically generated coherent acoustic phonons

Characterization of microstructure, chemistry and function of advanced energy materials remains a challenge for instrumentation science with tremendous opportunity for new discoveries. This active area of research is starting to make considerable strides with examples ranging from methodologies that employ bright X-rays, electron microscopy and optical spectroscopy. However, further development of instruments, capable of multimodal measurements, is necessary to fully reveal complex microstructure evolution in realistic environments and dynamical systems that are far from equilibrium. In this regard, laser-based instruments have a unique advantage as multiple measurement methodologies are easily combined into a single instrument using standard optics. A new pump-probe method that uses optically generated acoustic phonons is expanding standard optical characterization by providing depth resolved information. Here we report on a noteworthy extension of this pump-probe method to image grain microstructure in ceria. Rich information regarding the orientation of individual crystallites is obtained by monitoring acoustic phonon velocities and noting how the polarization of the probe beam influences the detected signal amplitude. When paired with other optical microscopies, this methodology will provide new perspectives for optical characterization of ceramic materials.

36 MATERIALS SCIENCE↗

BEYONDPLANCK XIII. Intensity foreground sampling, degeneracies, and priors

We present the intensity foreground algorithms and model employed within the BEYONDPLANCK analysis framework. The BEYONDPLANCK analysis is aimed at integrating component separation and instrumental parameter sampling within a global framework, leading to complete end-to-end error propagation in the Planck Low Frequency Instrument (LFI) data analysis. Given the scope of the BEYONDPLANCK analysis, a limited set of data is included in the component separation process, leading to foreground parameter degeneracies. In order to properly constrain the Galactic foreground parameters, we improve upon the previous Commander component separation implementation by adding a suite of algorithmic techniques. These algorithms are designed to improve the stability and computational efficiency for weakly constrained posterior distributions. These are: (1) joint foreground spectral parameter and amplitude sampling, building on ideas from MIRAMARE; (2) component-based monopole determination; (3) joint spectral parameter and monopole sampling; and (4) application of informative spatial priors for component amplitude maps. We find that the only spectral parameter with a significant signal-to-noise ratio using the current BEYONDPLANCK data set is the peak frequency of the anomalous microwave emission component, for which we find $ν$ p = 25.3 ± 0.5 GHz; all others must be constrained through external priors. Future works will be aimed at integrating many more data sets into this analysis, both map and time-ordered based, thereby gradually eliminating the currently observed degeneracies in a controlled manner with respect to both instrumental systematic effects and astrophysical degeneracies. When this happens, the simple LFI-oriented data model employed in the current work will need to be generalized to account for both a richer astrophysical model and additional instrumental effects. This work will be organized within the Open Science-based COSMOGLOBE community effort.

79 ASTRONOMY AND ASTROPHYSICS↗

A multimodal flow reactor for photocatalysis under atmospheric conditions

Photocatalysis is a promising concept for the direct conversion of solar energy into fuels and chemicals. The design, experimental protocol, and performance of a multimodal and versatile flow reactor for the characterization of powdered and immobilized photocatalysts are presented in this report. Ultimately, this instrument enables rigorous evaluation of photocatalysis performance metrics. The apparatus quantifies transient gas-phase reaction products via online real-time gas analyzer mass spectrometry (RTGA-MS). For H 2 , the most challenging gas, the photocatalytic system’s RTGA-MS gas detection sensitivity spans over three orders of magnitude and can detect down to tens of parts per million under atmospheric conditions. Using Pt nanoparticles supported on anatase TiO 2 photocatalyst via wet impregnation, the instrument’s capability for the characterization of photocatalytic H 2 evolution is demonstrated, resulting in an apparent quantum yield (AQY) of 48.1% ± 0.9% at 320 nm, 45.7% ± 0.3% at 340 nm and 31% ± 1% at 360 nm. The photodeposition of Pt on anatase TiO 2 was employed to demonstrate the instrument’s capability to track the transient behavior of photocatalysts, resulting in an improved 55% ± 2% AQY for H 2 evolution at 340 nm from aqueous methanol. This photocatalytic instrument enables systematic study of a wide variety of photocatalytic reactions such as water splitting and CO 2 reduction to valuable C2+ fuels and chemicals.

14 SOLAR ENERGY↗

Patient-Reported Outcomes in Pediatric Cancer Registration Trials: A US Food and Drug Administration Perspective

Pediatric patient-reported outcome (PRO) data can help inform the US Food and Drug Administration’s (FDA’s) benefit-risk assessment of cancer therapeutics by quantifying symptom and functional outcomes from the patient’s perspective. This study assessed use of PROs in commercial pediatric oncology trials submitted to the FDA for regulatory review. FDA databases were searched to identify pediatric oncology product applications approved between 1997 and 2020. Sponsor-submitted documents were reviewed to determine whether PRO data were collected, which instruments were used, and the quality of collected data (ie, sample size, completion rates, and use of fit-for-purpose instruments). The role of PROs in each trial (endpoint hierarchy) was also recorded in addition to whether any PRO endpoints were included in product labeling. We reviewed 17 pediatric oncology applications, 4 of which included PRO data: denosumab, tisagenlecleucel, larotrectinib, and selumetinib. In these 4 instances, PROs served as exploratory endpoints and were not incorporated in product labeling. Trials that collected PRO data were phase II or phase I/II single-arm studies with sample sizes of 28 to 88 patients. Symptomatic adverse events (AEs) were characterized using clinician-reported Common Terminology Criteria for Adverse Events (CTCAE) without additional patient self-report. PROs were infrequently used in pediatric cancer registration trials. When PROs were used, PRO data were limited by lack of a clear research objective and corresponding prospective statistical analysis plan. Contemporary PRO symptom libraries, such as the National Cancer Institute’s Pediatric PRO-CTCAE, may provide an opportunity to better evaluate the occurrence and impact of symptomatic AEs, from the patient’s perspective, in pediatric oncology trials.

Oncology↗

Biomechanical Analysis of Multilevel Posterior Cervical Spinal Fusion Constructs

Study Design: Controlled Laboratory Study Objective: To compare multilevel posterior cervical fusion (PCF) constructs stopping at C7, T1, and T2 under cyclic load to determine the range of motion (ROM) between the lowest instrumented level and lowest instrumented-adjacent level (LIV-1). Summary of Background Data: PCF is a mainstay of treatment for various cervical spine conditions. The transition between the flexible cervical spine and rigid thoracic spine can lead to construct failure at the cervicothoracic junction. There is little evidence to determine the most appropriate level at which to stop a multilevel PCF. Methods: Fifteen human cadaveric cervicothoracic spines were randomly assigned to 1 of 3 treatment groups: PCF stopping at C7, T1, or T2. Specimens were tested in their native state, following a simulated PCF, and after cyclic loading. Specimens were loaded in flexion-extension), lateral bending, and axial rotation. Three-dimensional kinematics were recorded to evaluate ROM. Results: The C7 group had greater flexion-extension motion than the T1 and T2 groups following instrumentation (10.17±0.83 degree vs. 2.77±1.66 degree and 1.06±0.55 degree, P <0.001), and after cyclic loading (10.42±2.30 degree vs. 2.47±0.64 degree and 1.99±1.23 degree, P <0.001). There was no significant difference between the T1 and T2 groups. The C7 group had greater lateral bending ROM than both thoracic groups after instrumentation (8.81±3.44 degree vs. 3.51±2.52 degree, P =0.013 and 1.99±1.99 degree, P =0.003) and after cyclic loading. The C7 group had greater axial rotation motion than the thoracic groups (4.46±2.27 degree vs. 1.26±0.69 degree, P =0.010; and 0.73±0.74 degree, P =0.003) following cyclic loading. Conclusion: Motion at the cervicothoracic junction is significantly greater when a multilevel PCF stops at C7 rather than T1 or T2. This is likely attributable to the transition from a flexible cervical spine to a rigid thoracic spine. Although this does not account for in vivo fusion, surgeons should consider extending multilevel PCF constructs to T1 when feasible. Level of Evidence: Not applicable.

Neurosciences & Neurology↗

Normality of I-V Measurements Using ML

There is an increased interest in instrument-computing ecosystems (ICEs) that support science workflows empowered by AI-automated experiments and computations in diverse areas. In particular, electrochemistry ICEs are promising for accelerating the design and discovery of electrochemical systems for energy storage and conversion, by automating significant parts of workflows that combine synthesis and characterization experiments with computations. They require the integration of flow controllers, solvent containers, pumps, fraction collectors, and potentiostats, all connected to an electrochemical cell, as illustrated in Fig. 1. These are specialized instruments with custom software that is not originally designed for network integration. We developed network and software solutions for electrochemical workflows that adapt system and instrument settings in real-time for multiple rounds of experiments. In particular, we developed Python wrappers for Application Programming Interfaces (APIs) of instrument commands and Pyro client-server modules that enable them to be executed from remote computers. The entire workflow is orchestrated by a Jupyter notebook running on a remote computer.

Al Najjar, Anees↗

Enabling Autonomous Electron Microscopy for Networked Computation and Steering

Advanced electron microscopy workflows require an ecosystem of microscope instruments and computing systems possibly located at different sites to conduct remotely steered and automated experiments. Current workflow executions involve manual operations for steering and measurement tasks, which are typically performed from control workstations co-located with microscopes; consequently, their operational tempo and effectiveness are limited. We propose an approach based on separate data and control channels for such an ecosystem of Scanning Transmission Electron Microscopes (STEM) and computing systems, for which no general solutions presently exist, unlike the neutron and light source instruments. We demonstrate automated measurement transfers and remote steering of Nion STEM physical instruments over site networks. We propose a Virtual Infrastructure Twin (VIT) of this ecosystem, which is used to develop and test our steering software modules without requiring access to the physical instrument infrastructure. Additionally, we develop a VIT for a multiple laboratory scenario, which illustrates the applicability of this approach to ecosystems connected over wide-area networks, for the development and testing of software modules and their later field deployment.

Al Najjar, Anees↗

Resource Management for Processing Wide Area Data Streams on Supercomputers

Modern scientific instruments generate enormous amount of data. Typically, the data collected from the instruments are stored in one or more files that are then moved to a distant supercomputer for processing. The final results are sent back to the user. In order to make effective use of the time on expensive instruments, experimenters want to process the data as they are generated. They want to stream the data from instruments' memory directly to a supercomputer's memory for analysis. Since the compute nodes in a supercomputer are not connected directly to the wide area network, the data streams need to be passed through intermediate gateway nodes. As opposed to the best effort file transfers, data streaming applications require resources at a specific time for a specific period. In this paper, we present a system model for enabling data streaming through gateway nodes and an algorithm to efficiently allocate gateway node resources along with compute nodes. We evaluate the algorithm using real-world traces on the Chameleon Cloud. The results show that our system can schedule compute and gateway resources efficiently for streaming analysis.

data streaming↗

In-flight performance of the XRISM/Resolve detector system

The Resolve instrument was launched on board the XRISM observatory in early September 2023. The Resolve spectrometer is based on a high-sensitivity X-ray calorimeter detector system (DS) that has been successfully deployed in many ground and sub-orbital spectrometers. However, the Resolve instrument is the first long-term implementation in space. The instrument will provide essential diagnostics for nearly every class of X-ray emitting objects, from galactic supernova remnants to the outskirts of galaxy clusters, without degradation for spatially extended objects. The Resolve DS consists of a 36-pixel microcalorimeter array operated at a heat sink temperature of 50 mK. In pre-flight testing, the DS demonstrated a resolving power of better than 1300 at 6 keV with a simultaneous bandpass from below 0.3 keV to above 12 keV and a timing precision better than 100μs. An anti-coincidence detector placed directly behind the microcalorimeter array effectively suppresses background. The detector energy-resolution budget included terms for interference from the Resolve cooling system and the spacecraft. Additional terms for energy-scale stability, on-orbit effects, and use of mid-grade events were also included, predicting an end-of-life, on-orbit performance for high- and mid-resolution grade events that meet the requirement of 7 eV FWHM at 6 keV. Here, we discuss the actual on-orbit performance of the Resolve DS and compare this with the performance in pre-flight testing, on-orbit predictions, and the almost identical Hitomi/SXS instrument. We will also discuss the on-orbit gain stability, an assessment of on-orbit interference, and measurements of the on-orbit background.

Astronomy and AstroPhysics↗

Revised astrometric calibration of the Gemini Planet Imager

We present a revision to the astrometric calibration of the Gemini Planet Imager (GPI), an instrument designed to achieve the high contrast at small angular separations necessary to image substellar and planetary-mass companions around nearby, young stars. We identified several issues with the GPI data reduction pipeline (DRP) that significantly affected the determination of the angle of north in reduced GPI images. As well as introducing a small error in position angle measurements for targets observed at small zenith distances, this error led to a significant error in the previous astrometric calibration that has affected all subsequent astrometric measurements. We present a detailed description of these issues and how they were corrected. We reduced GPI observations of calibration binaries taken periodically since the instrument was commissioned in 2014 using an updated version of the DRP. These measurements were compared to observations obtained with the NIRC2 instrument on Keck II, an instrument with an excellent astrometric calibration, allowing us to derive an updated plate scale and north offset angle for GPI. This revised astrometric calibration should be used to calibrate all measurements obtained with GPI for the purposes of precision astrometry.

79 ASTRONOMY AND ASTROPHYSICS↗

First flight performance of the Micro-X microcalorimeter X-ray sounding rocket

The flight of the Micro-X sounding rocket on July 22, 2018, marked the first operation of transition-edge sensors and their superconducting quantum interference device readouts in space. Here, the instrument combines the microcalorimeter array with an imaging mirror to take high-resolution spectra from extended X-ray sources. The first flight target was the Cassiopeia A supernova remnant. Although a rocket pointing malfunction led to no time on-target, data from the flight were used to evaluate the performance of the instrument and demonstrate the flight viability of the payload. The instrument successfully achieved a stable cryogenic environment, executed all flight operations, and observed X-rays from the on-board calibration source. The flight environment did not significantly affect the performance of the detectors compared with ground operation. The flight provided an invaluable test of the impact of external magnetic fields and the instrument configuration on detector performance. This flight provides a milestone in the flight readiness of these detector and readout technologies, both of which have been selected for future X-ray observatories.

79 ASTRONOMY AND ASTROPHYSICS↗

The Mini Astrophysical MeV Background Observatory (MAMBO) CubeSat mission

The origin of the cosmic diffuse gamma-ray (CDG) background in the 0.3 – 30 MeV energy range is a mystery that has persisted for over 40 years. The Mini Astrophysical MeV Background Observatory (MAMBO) is a CubeSat mission concept motivated by the fact that, since the MeV CDG is relatively bright, only a small detector is required to make highquality measurements of it. Indeed, the sensitivity of space-based gamma-ray instruments to the CDG is limited not by size, but by the locally generated instrumental background produced by interactions of energetic particles in spacecraft materials. Comparatively tiny CubeSat platforms provide a uniquely quiet environment relative to previous gamma-ray science missions. The MAMBO mission will provide the best measurements ever made of the MeV CDG spectrum and angular distribution, utilizing two key innovations: 1) low instrumental background on a 12U CubeSat platform; and 2) an innovative shielded spectrometer design that simultaneously measures signal and background. We describe the MAMBO instrument and mission concept in detail, including simulations and laboratory measurements demonstrating the key measurement concept.

Astronomy and astrophysics↗

Data for Clumping Index Estimation With 30°-tilted Cameras in Row Crops: Evaluation of Methods and Segment Size Effects

The clumping index (CI) quantifies the spatial distribution of foliage elements and is essential for accurately estimating the plant area index (PAI), canopy radiative transfer, and photosynthesis. Traditionally, the finite-length averaging method (LX), the gap size distribution method (CC), and a combined approach of CC and LX (CLX) have been applied to instruments like TRAC and digital hemispherical photography to estimate CI. However, a comprehensive evaluation of these methods in row crops remains limited, especially regarding the influence of segment size on CI. Meanwhile, digital cameras offer a cost-effective and user-friendly solution for canopy measurements in row crops, yet their application in this context remains underexplored. In this study, we employed a new approach using a 30°-tilted digital camera to estimate CI in corn and soybean fields, applying the LX, CC, and CLX methods. We systematically assessed the performance of these three methods by combining field measurements in real-world fields with simulations using the LESS 3D radiative transfer model. Our results showed that CLX applied to the whole image and 45° segment offered accurate estimation of CI (bias within ±0.1, RMSE < 0.2) and PAI (bias within ±0.4, RMSE < 1) in real-world fields and LESS simulations. The accuracy of the LX method was highly sensitive to segment size, with the best performance observed at the 15° segment (PAI bias within ±0.4). In contrast, the CC method remained stable across different segment sizes, and its performance was generally comparable to that of LX, except at the 15° segment. Across view zenith angles, CI derived from CC generally showed a continuous increase, while those from LX and CLX followed a rising trend at small zenith angles but began to decline at 68°, likely due to an increasing proportion of no-gap segments. Seasonally, LX tended to show decreasing CI during early growth stages but increased as the canopy matured, whereas CC and CLX showed gradually increasing CI before plateauing at peak PAI. The 30°-tilted camera effectively captured CI variations across different angles and growth stages, making it a practical and robust instrument for row crop canopy structure analysis. Applying these CI methods to digital cameras offers a low-cost and accessible CI estimation alternative, improving canopy structure monitoring accuracy in row crops.

Modeling↗