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At least 253 records · Page 14

Rare Earth Desorption Test with Citrate and Bicarbonate

LBT (lanthanide binding tag) cells were grown overnight in LB media with 0.05% Amp. 1:100 subculture taken from overnights, grown for 2 hours. LBT was induced with 0.002% arabinose added for 3 hours. REE adsorption was done by combining 350 ul (0.25% 1M MES, 12.5 uM Tb, and 12.5 uM La or Cu in sterile DI water) and 350 ul (LBT cells with OD = 1 in 10 mM MES), reacted for approx. 30 min. Following adsorption, citrate and bicarbonate solutions were used in desorption to recover rare earth from cell surface, and to further separate REE from non-REEs. The samples were then centrifuged and a fraction of the supernatant was collected for ICP-MS analysis.

15 GEOTHERMAL ENERGY↗

Single Component Sorption-Desorption Test Experimental Design Approach Discussions

A task was identified within the fission-product-transport work package to develop a path forward for doing testing to determine behavior of volatile fission products behavior and to engage members of the NGNP community to advise and dissent on the approach. The following document is a summary of the discussions and the specific approaches suggested for components of the testing. Included in the summary isare the minutes of the conference call that was held with INL and external interested parties to elicit comments on the approaches brought forward by the INL participants. The conclusion was that an initial non-radioactive, single component test will be useful to establish the limits of currently available chemical detection methods, and to evaluated source-dispersion uniformity. In parallel, development of a real-time low-concentration monitoring method is believed to be useful in detecting rapid dispersion as well as desorption phenomena. Ultimately, the test cycle is expected to progress to the use of radio-traced species, simply because this method will allow the lowest possible detection limits. The consensus of the conference call was that there is no need for an in-core test because the duct and heat exchanger surfaces that will be the sorption target will be outside the main neutron flux and will not be affected by irradiation. Participants in the discussion and contributors to the INL approach were Jeffrey Berg, Pattrick Calderoni, Gary Groenewold, Paul Humrickhouse, Brad Merrill, and Phil Winston. Participants from outside the INL included David Hanson of General Atomics, Todd Allen, Tyler Gerczak, and Izabela Szlufarska of the University of Wisconsin, Gary Was, of the University of Michigan, Sudarshan Loyalka and Tushar Ghosh of the University of Missouri, and Robert Morris of Oak Ridge National Laboratory.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

In-Situ Laser-Induced-Desorption-Spectroscopy Diagnostic Deployment on the Linear Plasma Device CSDX

A calibrated laser induced desorption diagnostic (LIDS) concept is developed under this award for application to fusion relevant plasma materials interactions studies. Small areal amounts of hydrogenic release from a deuterium filled PMI target are measured and quantified when irradiated by a LID flash heat event on the target surface. Good success was demonstrated by this project with the PISCES-E rf plasma device at UCSD by fully quantified measurement and removal of D from W-D co-deposit layers in experiments. However, adapting the LIDS technique to D plasma exposed W targets in the linear plasma CSDX device, now labelled PISCES-Rf, was prone to several technical challenges ranging from target line of sight access, laser focusing, and loss of optical spectroscopic signal strength in the larger PISCES-Rf vacuum system. The results are summarized in this report.

08 HYDROGEN↗

Light-Dependent Changes in the Spatial Localization of Metabolites in Solenostemon scutellarioides (Coleus Henna) Visualized by Matrix-Free Atmospheric Pressure Electrospray Laser Desorption Ionization Mass Spectrometry Imaging

The visualization of foliage color in plants provides immediate insight into some of the compounds that exist in the leaf. However, many non-colored compounds are also present; their cellular distributions are not readily identifiable optically. In this study we evaluate the applicability of mass spectrometry imaging (MSI) via electrospray laser desorption ionization (ELDI) to reveal the spatial distribution of metabolites. ELDI-MSI is a matrix free, atmospheric pressure ionization method that utilizes a UV laser coupled with supplemental ionization by electrospray. We specifically applied ELDI-MSI to determine the spatial distribution of metabolites in Coleus Henna half leaves that were grown with half-sections either fully illuminated or shaded. We monitored dynamic changes in the spatial distribution of metabolites in response to the change of illumination every 7 days for a 28 day period. A novel source-sink relationship was observed between the 2 halves of the experimental leaf. Furthermore, Coleus Henna leaves present visually recognizable sectors associated with the differential accumulation of flavonoids. Thus, we correlated the effect of differential illumination and presence or absence of flavonoids with metabolic changes revealed by the accumulation of carbohydrates, amino acids, and organic acids. Here, the results show the potential of ELDI-MSI to provide spatial information for a variety of plant metabolites with little sample preparation.

Coleus (Solenostemon scuttellarioides)↗

GOAmazon Thermal Desorption Chemical Ionization Mass Spectrometer

Ion abundance measured by Thermal Desorption Chemical Ionization Mass Spectrometer (using quadrupole mass spectrometer) Data file format: Column 1: date and time (UTC) Column 2: measurement uncertainty (units: integrated ion counts) Column 3: ion intensity (units: integrated ion counts) Column 4: 1 min SO2 mixing ratio in ppb Measurement uncertainty is +/- 0.2 ppb.

54 ENVIRONMENTAL SCIENCES↗

Particle composition measurements for ultrafine particles collected at the EPCAPE Mount Soledad site from 04-27-2023 to 06-13-2023 using a Thermal Desorption Chemical Ionization Mass Spectrometer

The dataset contains particle composition data for both the positive and negative reagent ion modes of the Thermal Desorption Chemical Ionization Mass Spectrometer (TDCIMS). The dataset is split into two directories: one for particles with diameters of 30 nm and the other for particles with diameters of less than 100 nm. The positive reagent ion mode uses H3O+ as the reagent ion, and ionization usually occurs through hydrogen addition. The negative mode uses O2- as the reagent ion. Negative mode ionization generally occurs through hydrogen abstraction, but O2- addition is also possible. Ion concentrations were normalized to total ion counts, and unknown ions were then removed from the data. The name of each ion fraction time series includes the mass to charge ratio and the chemical formula for the ion. Time is recorded in seconds since 1/1/1904. The time zone is UTC.

54 ENVIRONMENTAL SCIENCES↗

Hydrogen Desorption and Adsorption Measurements on Graphite Nanofibers

Graphite nanofibers were synthesized and their hydrogen desorption and adsorption properties are reported for 77 and 300 K. Catalysts were made by several different methods including chemical routes, mechanical alloying and gas condensation.

graphite nanofibers hydrogen desorption adsorption↗

Demonstration Testing of a Thermal Desorption Unit to Receive and Treat Waste with Unlimited Concentration of PCBs - 13437

For the last nine years, EnergySolutions and TD*X Associates LP have teamed up to provide the most comprehensive organic removal treatment process in the radioactive waste industry. The high performance thermal desorption unit (HP-TDU) located at the EnergySolutions Clive facility in Utah has successfully processed over 1,850 tons of organically contaminated radioactive mixed waste. Products from the HP-TDU system include a radioactively contaminated dry solid material that can be disposed in the on-site landfill and an organic condensate with high thermal energy content that is generally below background radiation and capable of free-release to a non-radioactive incinerator. Over the years, Permits and approvals have been obtained through the state of Utah, United States Environmental Protection Agency (USEPA) Region 8, and USEPA headquarters that enable the treatment of several waste categories including volatile and semi-volatile organic compounds, combustion-coded (CMBST) compounds, volatile metals, and polychlorinated biphenyls (PCBs). The unit has recently successfully completed Demonstration Testing for PCB concentrations up to 660,000 ppm (parts per million). Solid processed material from this Demonstration Testing was less than two ppm PCBs in three separate treatment runs; reprocessing or additional treatment was not needed to meet this limit. Through post-demonstration permitting, the system is unlimited in scope as approval has been given to receive and solidify up to pure PCBs down to this processing limit concentration to complete treatment of mixed waste. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Molecular Characterization of S- and N-containing Organic Constituents in Ambient Aerosols by negative ion mode High-Resolution Nanospray Desorption Electrospray Ionization Mass Spectrometry: CalNex 2010 field study

Samples of ambient aerosols from the 2010 California Research at the Nexus of Air Quality and Climate Change (CalNex) field study were analyzed using Nanospray Desorption Electrospray Ionization High Resolution Mass Spectrometry (nano-DESI/MS). Four samples per day were collected in Bakersfield, CA on June 20-24 with a collection time of 6 hours per sample. Four characteristic groups of organic constituents were identified in the samples: compounds containing carbon, hydrogen, and oxygen only (CHO), sulfur- (CHOS), nitrogen-(CHON), and both nitrogen- and sulfur-containing organics (CHONS). Within the groups, organonitrates, organosulfates, and nitroxy organosulfates were assigned based on accurate mass measurements and elemental ratio comparisons. Changes in the chemical composition of the aerosol samples were observed throughout the day. The number of observed CHO compounds increased in the afternoon samples, suggesting regional photochemical processing as a source. The average number of CHOS compounds had the smallest changes throughout the day, consistent with a more broadly distributed source. Both of the nitrogen-containing groups (CHON and CHONS) had greater numbers of compounds in the night and morning samples, indicating that nitrate radical chemistry was likely a source for those compounds. Most of the compounds were found in submicron particles. The size distribution of CHON compounds was bimodal. We conclude that the majority of the compounds observed were secondary in nature with both biogenic and anthropogenic sources.

Environmental Molecular Sciences Laboratory↗

Quantification of Brønsted Acid Sites in Zeolites by Water Desorption Thermogravimetry

The many studies that have been conducted on water adsorption on zeolites were carried out in “adsorption” mode, from adsorption isotherms or single-point measurements, with the samples being first degassed at high temperature, and then exposed to water vapor at variable partial pressure. Here, we report Thermogravimetric Analysis (TGA) studies of HZSM-5 saturated with water at room temperature, thus studying water adsorption in “desorption” mode. In this work, TGA was used to ascertain the amount of water remaining as a function of the pretreatment temperature, and to identify the temperature at which one water molecule per framework Al atom persists. Solid-state 1H NMR spectroscopy, combined with molecular modeling, provided evidence for water molecules hydrogen bonded to Brønsted acid sites and formation of oxonium species for distinct water per framework Al atom. TGA is shown to be a simple and expeditious technique to measure the number of Brønsted acid sites in aluminosilicate zeolites, with advantages over the traditional methods of IR or TPD of dangerous adsorbed ammonia or pyridine. TGA of adsorbed water also provides information on the water clusters formed at the acid sites of HZSM-5, which are proportional to the number of acid sites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Accelerated reactions in field desorption mass spectrometry

Field desorption mass spectrometry under ambient conditions is used to study solution-phase organic reactions in micro-volumes. Reagent solution is transferred onto the microdendrites of the field emitter, and reaction products are examined online by mass spectrometry. Three reactions, hydrazone formation by phenyl hydrazine and indoline-2,3-dione, the Katritzky reaction between a pyrylium salt and anisidine, and the Hantzsch synthesis of 1,4-dihydropyridine, were investigated, and reaction acceleration was observed to different extents. The increase in rate relative to the corresponding bulk reactions is attributed to solvent evaporation (simple concentration effect) and to the increase of surface-to-volume ratio (enhanced interfacial reactions). A distinguishing feature of this method of reaction acceleration, relative to that based on nano electrospray ionization, is the observation of radical cations and the formation of radical cation products. The research also breaks new ground in using field emitters at atmospheric pressure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Imaging of Lipids and Metabolites Using Nanospray Desorption Electrospray Ionization Mass Spectrometry

In recent years, mass spectroscopy imaging (MSI) has emerged as a foundational technique in metabolomics and drug screening providing deeper understanding of complex mechanistic pathways within biochemical systems and biological organisms. We have been invited to contribute a chapter to a new Springer series volume, entitled “Mass Spectrometry Imaging of Small Molecules”. The volume is planned for the highly successful lab protocol series Methods in Molecular Biology, published by Humana Press, USA. The volume is aimed to equip readers with step-by-step mass spectrometric imaging protocols and bring rapidly maturing methods of MS imaging to life science researchers. The chapter will provide a detailed protocol of ambient MSI by use of nanospray desorption electrospray ionization.

Lanekoff, Ingela↗