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DOE OSTI2024

Cellulose molecular weight of corn stover with cotreatment

Here we present a dataset of cellulose molecular weights from corn stover after a cotreatment process. The corn stover sample was subjected to a combination of mechanical disruption (ball milling) and consolidated bioprocessing (CBP) process using the bacterium C. thermocellum at 60 grams/L solids loadings. Cellulose was isolated from control, no cotreatment control, and cotreatment corn stover. Cellulose was then derivatized using anhydrous pyridine and phenyl isocyanate over 48 h at 70 ºC. The reaction was quenched by anhydrous methanol. Methanol and water mixture (7:3, v/v) was added dropwise to promote precipitation of the cellulose derivative. The solids were collected by filtration and thoroughly washed with the methanol and water mixture followed by water. The cellulose derivative was dried overnight under vacuum at 40°C. The obtained cellulose tricarbanilates was then dissolved in tetrahydrofuran (THF) at 1.0 mg/mL and the solution was filtered through a 0.45 µm PTFE filter and placed in an auto-sampler vial. The molecular weight of cellulose was measured by Agilent GPC SECurity 1200 system equipped with four Waters Styragel columns (i.e., HR0.5, HR2, HR4, and HR6) and a UV detector (270 nm). THF was used as the mobile phase. Data collection and processing was performed by Polymer Standards Service WinGPC Unity software (Build 6807). The molecular weight was calculated relative to the polystyrene calibration curve. The data on molecular weights provided information about the effects of cotreatment on corn stover cellulose molecular changes.

Cellulose, molecular weights, corn stover, cotreat↗

DOE OSTI2023

Editorial: Deep-sea observation equipment and exploration technology

The increasing interest in deep-sea exploration is a crucial catalyst for driving advancements in deep-sea observation technology research. Numerous sophisticated sensors have been developed to facilitate comprehensive studies in deep-sea physics, chemistry, and geology. For example, cutting-edge small and compact seabed samplers are now employed on various platforms, such as Autonomous Underwater Vehicles (AUVs), Remotely Operated Vehicles (ROVs), and Human-Operated Vehicles (HOVs), enabling observation of the hadal zone. Additionally, Micro-electromechanical systems (MEMS) sensors are routinely utilized for ocean wave observation. This Research Topic aims to foster new insights into ocean exploration and observation technology, including ocean sensor technology, ocean observation platforms, and ocean observation reliability technology.

47 OTHER INSTRUMENTATION↗

DOE OSTI2023

SARS-CoV-2 raw wastewater surveillance from student residences on an urban university campus

The COVID-19 pandemic brought about an urgent need to monitor the community prevalence of infection and detect the presence of SARS-CoV-2. Testing individual people is the most reliable method to measure the spread of the virus in any given community, but it is also the most expensive and time-consuming. Wastewater-based epidemiology (WBE) has been used since the 1960s when scientists implemented monitoring to measure the effectiveness of the Polio vaccine. Since then, WBE has been used to monitor populations for various pathogens, drugs, and pollutants. In August 2020, the University of Tennessee-Knoxville implemented a SARS-CoV-2 surveillance program that began with raw wastewater surveillance of the student residence buildings on campus, the results of which were shared with another lab group on campus that oversaw the pooled saliva testing of students. Sample collection began at 8 am, and the final RT-qPCR results were obtained by midnight. The previous day’s results were presented to the campus administrators and the Student Health Center at 8 am the following morning. The buildings surveyed included all campus dormitories, fraternities, and sororities, 46 buildings in all representing an on-campus community of over 8,000 students. The WBE surveillance relied upon early morning “grab” samples and 24-h composite sampling. Because we only had three Hach AS950 Portable Peristaltic Sampler units, we reserved 24-h composite sampling for the dormitories with the highest population of students. Samples were pasteurized, and heavy sediment was centrifuged and filtered out, followed by a virus concentration step before RNA extraction. Each sample was tested by RT-qPCR for the presence of SARS-CoV-2, using the CDC primers for N Capsid targets N1 and N3. The subsequent pooled saliva tests from sections of each building allowed lower costs and minimized the total number of individual verification tests that needed to be analyzed by the Student Health Center. Our WBE results matched the trend of the on-campus cases reported by the student health center. The highest concentration of genomic copies detected in one sample was 5.06 × 10 7 copies/L. Raw wastewater-based epidemiology is an efficient, economical, fast, and non-invasive method to monitor a large community for a single pathogen or multiple pathogen targets.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2023

Evaluating various composite sampling modes for detecting pathogenic SARS-CoV-2 virus in raw sewage

Inadequate sampling approaches to wastewater analyses can introduce biases, leading to inaccurate results such as false negatives and significant over- or underestimation of average daily viral concentrations, due to the sporadic nature of viral input. To address this challenge, we conducted a field trial within the University of Tennessee residence halls, employing different composite sampling modes that encompassed different time intervals (1 h, 2 h, 4 h, 6 h, and 24 h) across various time windows (morning, afternoon, evening, and late-night). Our primary objective was to identify the optimal approach for generating representative composite samples of SARS-CoV-2 from raw wastewater. Utilizing reverse transcription-quantitative polymerase chain reaction, we quantified the levels of SARS-CoV-2 RNA and pepper mild mottle virus (PMMoV) RNA in raw sewage. Our findings consistently demonstrated that PMMoV RNA, an indicator virus of human fecal contamination in water environment, exhibited higher abundance and lower variability compared to pathogenic SARS-CoV-2 RNA. Significantly, both SARS-CoV-2 and PMMoV RNA exhibited greater variability in 1 h individual composite samples throughout the entire sampling period, contrasting with the stability observed in other time-based composite samples. Through a comprehensive analysis of various composite sampling modes using the Quade Nonparametric ANCOVA test with date, PMMoV concentration and site as covariates, we concluded that employing a composite sampler during a focused 6 h morning window for pathogenic SARS-CoV-2 RNA is a pragmatic and cost-effective strategy for achieving representative composite samples within a single day in wastewater-based epidemiology applications. This method has the potential to significantly enhance the accuracy and reliability of data collected at the community level, thereby contributing to more informed public health decision-making during a pandemic.

sampling timing↗

DOE OSTI2022

Performing Bayesian Analyses With AZURE2 Using BRICK: An Application to the 7 Be System

Phenomenological R-matrix has been a standard framework for the evaluation of resolved resonance cross section data in nuclear physics for many years. It is a powerful method for comparing different types of experimental nuclear data and combining the results of many different experimental measurements in order to gain a better estimation of the true underlying cross sections. Yet a practical challenge has always been the estimation of the uncertainty on both the cross sections at the energies of interest and the fit parameters, which can take the form of standard level parameters. Frequentist (χ 2 -based) estimation has been the norm. In this work, a Markov Chain Monte Carlo sampler, emcee, has been implemented for the R-matrix code AZURE2, creating the Bayesian R-matrix Inference Code Kit (BRICK). Bayesian uncertainty estimation has then been carried out for a simultaneous R-matrix fit of the 3 He (α,γ) 7 Be and 3 He (α,α) 3 He reactions in order to gain further insight into the fitting of capture and scattering data. Both data sets constrain the values of the bound state α-particle asymptotic normalization coefficients in 7 Be. The analysis highlights the need for low-energy scattering data with well-documented uncertainty information and shows how misleading results can be obtained in its absence.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2024

Modeling PAH Mixture Interactions in a Human In Vitro Organotypic Respiratory Model

One of the most significant challenges in human health risk assessment is to evaluate hazards from exposure to environmental chemical mixtures. Polycyclic aromatic hydrocarbons (PAHs) are a class of ubiquitous contaminants typically found as mixtures in gaseous and particulate phases in ambient air pollution associated with petrochemicals from Superfund sites and the burning of fossil fuels. However, little is understood about how PAHs in mixtures contribute to toxicity in lung cells. To investigate mixture interactions and component additivity from environmentally relevant PAHs, two synthetic mixtures were created from PAHs identified in passive air samplers at a legacy creosote site impacted by wildfires. The primary human bronchial epithelial cells differentiated at the air–liquid interface were treated with PAH mixtures at environmentally relevant proportions and evaluated for the differential expression of transcriptional biomarkers related to xenobiotic metabolism, oxidative stress response, barrier integrity, and DNA damage response. Component additivity was evaluated across all endpoints using two independent action (IA) models with and without the scaling of components by toxic equivalence factors. Both IA models exhibited trends that were unlike the observed mixture response and generally underestimated the toxicity across dose suggesting the potential for non-additive interactions of components. Overall, this study provides an example of the usefulness of mixture toxicity assessment with the currently available methods while demonstrating the need for more complex yet interpretable mixture response evaluation methods for environmental samples.

3D in vitro models↗

DOE OSTI2023

Detecting and Characterizing Mg ii Absorption in DESI Survey Validation Quasar Spectra

Abstract We present findings of the detection of Magnesium II (Mg ii , λ = 2796, 2803 Å) absorbers from the early data release of the Dark Energy Spectroscopic Instrument (DESI). DESI is projected to obtain spectroscopy of approximately 3 million quasars (QSOs), of which over 99% are anticipated to be at redshifts greater than z > 0.3, such that DESI would be able to observe an associated or intervening Mg ii absorber illuminated by the background QSO. We have developed an autonomous supplementary spectral pipeline that detects these systems through an initial line-fitting process and then confirms the line properties using a Markov Chain Monte Carlo sampler. Based upon a visual inspection of the resulting systems, we estimate that this sample has a purity greater than 99%. We have also investigated the completeness of our sample in regard to both the signal-to-noise properties of the input spectra and the rest-frame equivalent width ( W 0 ) of the absorber systems. From a parent catalog containing 83,207 quasars, we detect a total of 23,921 Mg ii absorption systems following a series of quality cuts. Extrapolating from this occurrence rate of 28.8% implies a catalog at the completion of the five-year DESI survey that will contain over eight hundred thousand Mg ii absorbers. The cataloging of these systems will enable significant further research because they carry information regarding circumgalactic medium environments, the distribution of intervening galaxies, and the growth of metallicity across the redshift range 0.3 ≤ z < 2.5.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2026

Optimizing Optical Searches for Supermassive Black Hole Binaries in Active Galactic Nuclei Light Curves: Fourier versus Bayesian Periodicity Detection

Simulations predict that supermassive black hole binaries (SMBHBs) will exhibit periodic brightness variations that may exceed the stochastic variability intrinsic to active galactic nuclei (AGN). In this paper, we simulate SMBHBs with damped random walk (DRW) AGN variability and an added sinusoidal signal from the orbital motion, and test three methods—a generalized Lomb–Scargle periodogram (GLSP), a nested Bayesian sampler (NBS), and a weighted wavelet z-transform (or WWZ)—to determine which is best at recovering the periodicity. Our simulated light curves follow the properties of the Catalina Real-Time Transient Survey (or CRTS), Legacy Survey of Space and Time (LSST), and Zwicky Transient Facility (ZTF) to best inform current and future SMBHB searches. We map a broad range of parameter space and identify which DRW-only light curves best mimic periodicity and pass each method’s model selection. The NBS performs best at detecting periodicity and filtering out DRW-only light curves. Combined candidate selection with both the NBS and GLSP significantly reduces false-positive rates (FPRs) with marginal impact on true-positive rates (TPRs). With this joint model selection pipeline, we find the lowest FPRs in ZTF-like simulations and the highest detection rates in LSST-like simulations. Using a modified computation of the false-alarm probability with GLSP, we efficiently triage LSST AGN light curves (∼10 7 light curves in ∼10–30 hr) and achieve TPRs and FPRs of ∼40% and ∼0.5%, respectively.

Banaszak, Sebastian M. [Vanderbilt Univ., Nashvill↗

DOE OSTI2025

Seasonal investigation of ultrafine-particle organic composition in an eastern Amazonian rainforest

Abstract. Reports on the composition of ultrafine particles (<100 nm in diameter) in the Amazon are scarce, due in part to the fact that new-particle formation has rarely been observed near ground level. Ultrafine particles near the surface have nevertheless been observed, leaving open questions regarding the sources and chemistry of their formation and growth, particularly as these vary across seasons. Here, we present measurements of the composition of ultrafine particles collected in the Tapajós National Forest (2.857° S, 54.959° W) during three different seasonal periods: 10–30 September 2016 (SEP), 18 November–23 December 2016 (DEC), and 22 May–21 June 2017 (JUN). Size-selected (5–70 nm) particles were collected daily (for 22 h each day) using an offline sampler. Samples collected during the three time periods were compiled and analyzed using liquid chromatography coupled with Orbitrap high-resolution mass spectrometry. Our findings suggest a sustained influence of isoprene organosulfate chemistry on ultrafine particles from the different periods. We present chemical evidence that indicates that biological-spore fragmentation impacted ultrafine-particle composition during the late wet season (JUN), while chemical markers for biomass burning and secondary chemistry peaked during the dry season (SEP and DEC). Higher oxidation states and degrees of unsaturation were observed for organics in the dry season (SEP and DEC), suggesting greater extents of aerosol aging. Finally, applying a volatility parameterization to the observed compounds suggests that organic sulfur species are likely key drivers of new-particle growth in the region due to their low volatility compared to other species.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2023

Quantitative chemical assay of nanogram-level particulate matter using aerosol mass spectrometry: characterization of particles collected from uncrewed atmospheric measurement platforms

Abstract. Aerosol generation techniques have expanded the utility of aerosol mass spectrometry (AMS) for offline chemical analysis of airborne particles and droplets. However, standard aerosolization techniques require relatively large liquid volumes (e.g., several milliliters) and high sample masses that limit their utility. Here we report the development and characterization of a micronebulization AMS (MN-AMS) technique that requires as low as 10 µL of sample and can provide the quantification of the nanogram level of organic and inorganic substances via the usage of an isotopically labeled internal standard (34SO42-). Using standard solutions, the detection limits for this technique were determined at 0.19, 0.75, and 2.2 ng for sulfate, nitrate, and organics, respectively. The analytical recoveries for these species are 104 %, 87 %, and 94 %, respectively. This MN-AMS technique was applied successfully to analyze filter and impactor samples collected using miniature particulate matter (PM) samplers deployable on uncrewed atmospheric measurement platforms, such as uncrewed aerial systems (UASs) and tethered balloon systems (TBSs). Chemical composition of PM samples collected from a UAS field campaign conducted at the Department of Energy's (DOE) Southern Great Plains (SGP) observatory was characterized. The offline MN-AMS data compared well with the in situ PM composition measured by a co-located aerosol chemical speciation monitor (ACSM). In addition, the MN-AMS and ion chromatography (IC) agreed well for measurements of sulfate and nitrate concentrations in the PM extracts. This study demonstrates the utility of combining MN-AMS with uncrewed measurement platforms to provide quantitative measurements of ambient PM composition.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2024

Simulations of the collection of mesospheric dust particles with a rocket instrument

We investigate the collection of dust particles in the mesosphere with the MESS (MEteoric Smoke Sampler) instrument that is designed to fly on a sounding rocket. We assume that the ice particles that form in the polar mesosphere between 80 and 85 km altitude in summer contain meteoric smoke particles; and these should be collected with MESS. The instrument consists of a collection device with an opening and closure mechanism, as well as an attached conic funnel which increases the sampling area in comparison to the collection area. Dust particles are collected either directly after passing through the instrument or indirectly after colliding with and fragmenting on the funnel wall. We calculate the dust and fragment trajectories in the detector to determine the collection efficiency for different particle sizes, rocket velocities, and heights, and we find the final velocities and the temperatures of the particles. The considered design has a sampling area of 62.78 mm diameter and a collection area of 20 mm diameter. For the conditions at the rocket launch site in Andøya, Norway, we estimate the collection of meteoric smoke particles contained in the ice particles to be ~10 12 –10 14 amu mm –2 . The estimated temperatures suggest that the composition of these smoke particles is not affected by the collection. Our calculations also show that keeping the instrument open above 85 km altitude increases the amount of small smoke particles that are directly collected. The directly collected smoke particles are heated as they decelerate, which can affect their composition.

47 OTHER INSTRUMENTATION↗

DOE OSTI2025

A novel methodology for assessing the hygroscopicity of aerosol filter samples

Abstract. Due to US regulations, concentrations of hygroscopic inorganic sulfate and nitrate have declined in recent years, leading to an increased importance of the hygroscopic nature of organic matter (OM). The hygroscopicity of OM is poorly characterized because only a fraction of the multitude of organic compounds in the atmosphere is readily measured, and there is limited information on their hygroscopic behaviors. Hygroscopicity of aerosol is traditionally measured using a humidified tandem differential mobility analyzer (HTDMA) or electrodynamic balance (EDB). EDB measures water uptake by a single particle. For ambient and chamber studies, HTDMA measurements provide water uptake and particle size information but not chemical composition. To fill this information gap, we developed a novel methodology to assess the water uptake by particles collected on Teflon filters. This method uses the same filter sample for both hygroscopicity measurements and chemical characterization, thereby providing an opportunity to link the measured hygroscopicity with ambient particle composition. To test the method, hygroscopic measurements were conducted in the laboratory for ammonium sulfate, sodium chloride, glucose, and malonic acid, which were collected on 25 mm Teflon filters using an aerosol generator and sampler. Constant-humidity solutions (CHSs), including potassium chloride, barium chloride dihydrate, and potassium sulfate, were employed in a saturated form to maintain the relative humidity (RH) at approximately 84 %, 90 %, and 97 % in small chambers. Our preliminary experiments revealed that, without the pouch, water uptake measurements were not feasible due to rapid water loss during weighing. Additionally, we observed some absorption by the aluminum pouch itself. To account for this, concurrent measurements were conducted for both the loaded and the blank filters at each RH level. Thus, the dry loaded and blank Teflon filters were placed in aluminum pouches with one side open and in RH-controlled chambers for more than 24 h. The wet loaded samples and wet blanks were then weighed using an ultramicrobalance to determine the water uptake by the respective compound and the blank Teflon filter. The net amount of water absorbed by each compound was calculated by subtracting the water uptake of the blank filter from that of the wet loaded filter. Hygroscopic parameters, including the water-to-solute (W / S) ratio, molality, mass fraction solute (mfs), and growth factors (GFs), were calculated from the measurements. The results obtained are consistent with those reported by the Extended Aerosol Inorganics Model (E-AIM) and previous studies utilizing HTDMA and EDB for these compounds, highlighting the accuracy of this new methodology. This new approach enables the hygroscopicity and chemical composition of individual filter samples to be assessed so that in complex mixtures, such as chamber and ambient samples, the total water uptake can be parsed between the inorganic and organic components of the aerosol.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Understanding the relative importance of vertical and horizontal flow in ice-wedge polygons

Abstract. Ice-wedge polygons are common Arctic landforms. The future of these landforms in a warming climate depends on the bidirectional feedback between the rate of ice-wedge degradation and changes in hydrological characteristics. This work aims to better understand the relative roles of vertical and horizontal water fluxes in the subsurface of polygonal landscapes, providing new insights and data to test and calibrate hydrological models. Field-scale investigations were conducted at an intensively instrumented location on the Barrow Environmental Observatory (BEO) near Utqiaġvik, AK, USA. Using a conservative tracer, we examined controls of microtopography and the frost table on subsurface flow and transport within a low-centered and a high-centered polygon. Bromide tracer was applied at both polygons in July 2015 and transport was monitored through two thaw seasons. Sampler arrays placed in polygon centers, rims, and troughs were used to monitor tracer concentrations. In both polygons, the tracer first infiltrated vertically until encountering the frost table and was then transported horizontally. Horizontal flow occurred in more locations and at higher velocities in the low-centered polygon than in the high-centered polygon. Preferential flow, influenced by frost table topography, was significant between polygon centers and troughs. Estimates of horizontal hydraulic conductivity were within the range of previous estimates of vertical conductivity, highlighting the importance of horizontal flow in these systems. This work forms a basis for understanding complexity of flow in polygonal landscapes.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2021

CACTI ARM Mobile Facility (AMF) Measurements of Ice Nucleating Particles

The dataset comprises measures, using Colorado State University's Ice Spectrometer (IS, an immersion freezing device with a range from 0°C down to -26 to -29°C) of atmosperic ice nucleating particle (INP) concentrations taken on ARM's Mobile Facility (AMF-1) Aerosol Observing System, near Villa Yacanto in central Argentina, during the Cloud, Aerosol, and Complex Terrain Interactions (CACTI) Experiment. A filter sampler was mounted on the AOS trailer (2 m below the AOS inlet). Single-use filter units open to the atmosphere fitted with pre-cleaned and pre-sterilized, 47-mm dia. Nuclepore polycarbonate filters were used. Filters were typically drawn for an 8-hour period, totaling 6000 liters sampled on average. After collection, filters were stored at -20°C until processed. Initial processing to obtain spectra of INP number concentration active via the immersion freezing mechanism versus temperature was conducted using CSU's IS instrument (McCluskey et al., 2018). For measurment of INPs, collected aerosol particles were re-suspended in 7-8 mL of 0.1 µm-filtered deionized (DI) water. Aliquots of each suspension, and serial dilutions, were dispensed into trays which were fit into aluminum blocks in the IS. Samples are cooled at 0.33°C min-1 and the freezing temperatures of wells recorded automatically. Cumulative INP concentrations were determined by first calculating the INPs per mL of suspension based on Vali (1971) and then converting to concentration per standard liter of air using the proportion of the total liquid sample dispensed and the air sample volumes. An aliquot of suspension fro selected samples were also heat treated (95°C for 20 min) to denature and deactivate biological INPs, and another aliquot digested in 10% H2O2 at 95°C under UV-B to remove all organic carbon INPs. McCluskey, C. S., J. Ovadnevaite, M. Rinaldi, J. Atkinson, F. Belosi, D. Ceburnis, S. Marullo, T. C. J. Hill, U. Lohmann, Z. A. Kanji, C. O’Dowd, S. M. Kreidenweis, P. J. DeMott, 2018: Marine and Terrestrial Organic Ice Nucleating Particles in Pristine Marine to Continentally-Influenced Northeast Atlantic Air Masses, Journal of Geophysical Research: Atmospheres, 123, 6196–6212, https://doi.org/10.1029/2017JD028033. Vali, G., 1971: Quantitative evaluation of experimental results on the heterogeneous freezing nucleation of supercooled liquids. J. Atmos. Sci., 28, 402–409.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

AEROICESTUDY-Colorado State University Ice Spectrometer

The dataset comprises measures, using Colorado State University's Ice Spectrometer (IS, an immersion freezing device with a range from 0 °C down to -26 to -29 °C) of atmospheric ice nucleating particle (INP) concentrations taken at ARM's Southern Great Plains (SGP) Site Guest Instrument Facility (GIF), in Lamont, Oklahoma, during the Aerosol-Ice Formation Closure Pilot Study (AEROICESTUDY). A filter sampler was mounted approximately 6 m above ground level atop the GIF rooftop platform. Single-use filter units open to the atmosphere fitted with pre-cleaned and pre-sterilized, 47-mm diameter Nuclepore polycarbonate filters were used. Filters were typically drawn for either a full day period (9AM-5PM CDT) or broken up into morning (9AM-12PM CDT) and afternoon (1PM-5PM CDT) periods. Additionally, 4 overnight filters were taken (6PM-8AM CDT). The volume of air filtered was typically between 3000 and 8000 standard liters for daily samples. After collection, filters were stored at -20 °C until processed. Initial processing to obtain spectra of INP number concentration active via the immersion freezing mechanism versus temperature was conducted using CSU's IS instrument (McCluskey et al., 2018). For measurement of INPs, collected aerosol particles were re-suspended in 8 mL of 0.1 µm-filtered deionized (DI) water. Aliquots of each suspension, and serial dilutions, were dispensed into trays which were fit into aluminum blocks in the IS. Samples were cooled at 0.33 °C per min and the freezing temperatures of wells recorded automatically. Cumulative INP concentrations were determined by first calculating the INPs per mL of suspension based on Vali (1971) and then converting to concentration per standard liter of air using the proportion of the total liquid sample dispensed and the air sample volumes. Two-tailed, 95% confidence intervals for binomial sampling were based on Equation 2 from Agresti and Coull (1998). Aliquots of suspensions from selected samples were also heat treated (95 °C for 20 min) to denature and deactiv

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2024

MOSAiC-Colorado State University Ice Spectrometer

This data set contains atmospheric ice nucleating particle (INP) measurements, using Colorado State University’s (CSU) Ice Spectrometer (IS), of filter collections taken at the U.S. DOE ARM AMF2 site onboard the R/V Polarstern P-deck during the Multidisciplinary Drifting Observatory for the Study of Arctic Climate (MOSAiC) field campaign. Samples were collected from October 27, 2019 to September 24, 2020. A filter sampler was mounted approximately 15 m above ground level on a railing in proximity to (and approximately 3 m below) the Aerosol Observation System (AOS) inlet. Single-use filter units open to the atmosphere were pre-cleaned and pre-loaded with 47-mm diameter Nuclepore polycarbonate (0.2 µm pore-diameter) filters. Filters were typically drawn for a three-day period, with an average volume of air filtered of 87,000 standard liters. Total volumes were calculated through recorded daily flow rates using a mass flow meter (TSI). After collection, filters were stored and transported frozen until analysis using CSU’s IS instrument (McCluskey et al., 2018). Aerosol particles were first re-suspended in 8 mL of 0.1 µm-filtered deionized (DI) water. Aliquots of each suspension, and corresponding 11-fold dilutions, were dispensed into polymerase chain reaction (PCR) trays and placed into the aluminum blocks of the IS. Samples were cooled at approximately 0.33 °C min -1 and freezing detected optically with corresponding temperatures recorded. Cumulative INP concentrations were determined through calculating the number of INPs per mL of suspension (Vali, 1971) and converting to concentration per standard L of air by accounting for the proportion of liquid used and volume of air collected. All samples were corrected for the number of INPs on the average of four field blanks (cleaned, handled, transported, and analyzed in the same way without air flow). Two-tailed, 95% confidence intervals for binomial sampling are provided (Agresti and Coull, 1998). Select samples were also heat treated (95 °C for 20 min) to denature and deactivate biological INPs present and digested in 10% H 2 O 2 at 95 °C under UV-B for 20 min to remove any organic carbon INPs. Agresti, A, and BA Coull. 1998. "Approximate is better than “exact” for interval estimation of binomial proportions." American Statistics 52: 119–126. https://doi.org/10.2307/2685469 McCluskey, CS, J Ovadnevaite, M Rinaldi, J Atkinson, F Belosi, D Ceburnis, … and PJ DeMott. 2018. "Marine and Terrestrial Organic Ice-Nucleating Particles in Pristine Marine to Continentally Influenced Northeast Atlantic Air Masses." Journal of Geophysical Research: Atmospheres 123 (11): 6196–6212, https://doi.org/10.1029/2017JD028033 Vali, G. 1971. "Quantitative Evaluation of Experimental Results and the Heterogeneous Freezing Nucleation of Supercooled Liquids." Journal of the Atmospheric Sciences 28: 402-209. https://doi.org/10.1175/1520-0469(1971)028<0402:QEOERA>2.0.CO;2

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2023

Ice nucleation measurements from DRUM impactors during TRACER campaign in the Houston TX region from July to September 2022

During TRACER, three Davis Rotating Uniform size-cut Monitors (DRUM; DRUMAir 4-DRUM) were used to collect aerosols for ice nucleation measurements in the Brooks laboratory at Texas A&M University. The three instruments were located at AMF1 in La Porte, Ancillary site in Guy (ANC), and onboard the Texas A&M Rapid Onsite Atmospheric Measurements Van (ROAM-V). ROAM-V was deployed to capture airmasses behind (maritime) and ahead (continental) of the passage of the sea-breeze front through Houston. On select sampling days, ROAM-V sampled in the morning/mid-day on the coast and then transited to a second inland site for the afternoon/evening. The suite of instruments deployed on ROAM-V included a Condensation Particle Counter (CPC; GRIMM Model 5.403 CPC), Scanning Mobility Particle Sizer (SMPS; TSI 3750 detector, TSI 3082 classifier, TSI 3088 neutralizer, TSI 3081A Differential Mobility Analyzer), Cloud Condensation Nuclei counter (Droplet Measurement Technologies CCN Counter), micro pulse lidar (Droplet Measurement Technologies Micro Pulse LiDAR (miniMPL)), and one of the Davis Rotating Uniform size-cut Monitors (DRUM; DRUMAir 4-DRUM). Before sampling at each location, the latitude and longitude were recorded using the GPS on the phone application “My Altitude”. Each DRUM sampler was operated at a flow rate of 23 LPM. Each DRUM has four stages where the aerodynamic diameter size cuts are as follows: stage 1 larger than 3 μm, stage 2 from 3 to 1.2 μm, stage 3 from 1.2 to 0.34 μm, and stage 4 from 0.34 to 0.15 μm. Pretreated aluminum foil was used as a substrate on all stages. At AMF1 and ANC sites, the DRUMs were operated on the shared aerosol inlet, with generous support of the DOE ARM site staff. These instruments rotated 24 mm per day and only contained aluminum foil substrates. Substrates were changed weekly and transported to Texas A&M for storage in -80C freezer until analysis. The DRUM onboard ROAM-V was operated at a faster rotation rate of 150 mm per day to clearly separate the multiple deployment locations for ROAM-V. For the ROAM-V DRUM, substrates were changed every deployment and transported to Texas A&M for storage in -80C freezer until analysis. At Texas A&M, ice nucleation experiments were conducted to measure the ice nucleation temperature of the ambient aerosol samples collected from the three DRUMs using our previously established procedures (Alsante et al., 2023; Fornea et al., 2009; Matthews et al., 2023). For ice nucleation, only samples collected on stage 3 were analyzed, given that these are the most relevant size (1.2 to 0.34 μm diameter) for potential ice nucleating particles. For the AMF1 and ANC sites, we cut and analyzed 2 mm (2-hour) samples. We analyzed the time periods of the AMF1 site instrument when the ROAM-V was deployed. A 72-hour period from July 11th at 23:49 through July 15th at 1:49 was analyzed from the ANC site instrument. For the ROAM-V instrument, we separated the daily samples by site location. Between 1- and 6-hour independent samples were analyzed at each location. We also cut the ROAM-V samples in half to allow for compositional analysis of the aerosol on the other half of the substrate. All viable samples from the ROAM-V were analyzed. Analysis was done using a custom-built ice nucleation apparatus, recently updated to include an array of 16 individual samples (Matthews et al., 2023). On our experimental setup, we used 100 μL of Ultra-High-Performance Liquid Chromatography (UHPLC) water (Sigma Aldrich, >99.9% purity) to wash off the aerosol from the DRUM substrate. Then, we micropipetted 2 μL droplet samples into each of the 16 wells of the array, using hydrophobically coated microscope slides. Experiments would cycle 28 times from 10 C to -40C over a 20-hour period. During analysis of the TRACER samples, nine experiments were conducted with UHPLC water process blanks that followed an identical preparation procedure. The average freezing temperature and standard deviation for these process blanks is -27.7±2.4 C. This data was collected for ARM Field Campaign AFC07023 and supported by DOE ASR grant DE-SC0021047. For any further questions, please feel free to contact the instrument PI, Sarah D. Brooks, sbrooks@tamu.edu. Alsante, A. N., Thornton, D. C., & Brooks, S. D. (2023). Ice nucleation catalyzed by the photosynthesis enzyme RuBisCO and other abundant biomolecules. Communications Earth & Environment, 4(1), 51. Fornea, A. P., Brooks, S. D., Dooley, J. B., & Saha, A. (2009). Heterogeneous freezing of ice on atmospheric aerosols containing ash, soot, and soil. Journal of Geophysical Research: Atmospheres, 114(D13). DOI:10.1029/2009JD011958 Matthews, B. H., Alsante, A. N., & Brooks, S. D. (2023). Pollen Emissions of Subpollen Particles and Ice Nucleating Particles. ACS Earth and Space Chemistry.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2025

SCILLA 1 Hz merged data

The overarching goal of the Southern California Interactions of Low Cloud and Land Aerosol (SCILLA) experiment is to understand the interplay among horizontal circulation, vertical mixing, aerosols and clouds in the Southern California (SoCal) Bight. Eddy circulations within the Bight are frequently present when low clouds are persistent, and the transport of pollution into the Bight also depends on the regional and local circulation. The contrast between the cooler near-surface marine air with the warmer overlying continental and/or free tropospheric air is crucial to the efficiency of vertical mixing, and vertical transport of aerosols into the boundary layer. The CIRPAS Twin Otter aircraft was based in San Diego, CA, to perform airborne measurements of winds, aerosols, and clouds for 1 month (June 2023), with a geographical focus on the SoCal Bight. The deployment coincided with the DOE-funded Eastern Pacific Cloud Aerosol Precipitation Experiment (EPCAPE), which deployed a range of ground-based aerosol and cloud sensors and samplers from Feb. 2023 to Feb. 2024, mostly in and around San Diego. The aircraft deployment specifically seeks to answer questions about the cause of regions of elevated cloud drop number concentration from satellite-observed variations over the SoCal Bight, the role of horizontal advection relative to vertical transport and mixing, and the role of the thermodynamic properties (rather than aerosol properties) of continental air in modifying nearshore clouds.

54 ENVIRONMENTAL SCIENCES↗