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At least 109 records · Page 6

Solvent Hold Tank Sample Results for MCU-16-348-349-350: March 2016 Monthly Sample

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-348-349-350), pulled on 03/30/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-348-349-350 indicated the Isopar TM L concentration is above its nominal level (101%). The modifier (CS-7SB) and the TiDG concentrations are 9% and 55% below their nominal concentrations. This analysis confirms the solvent may require the addition of TiDG, and possibly of modifier. Based on the current monthly sample, the levels of TiDG, Isopar TM L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Solvent Hold Tank Sample Results for MCU-16-596-597-598: April 2016 Monthly Sample

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-596-597-598), pulled on 04/30/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-596-597-598 indicated the Isopar™L concentration is above its nominal level (102%). The modifier (CS-7SB) is 14% below its nominal concentration, while the TiDG and MaxCalix concentrations are at and above their nominal concentrations, respectively. This analysis confirms the solvent may require the addition of modifier. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Solvent Hold Tank Sample Results for MCU-16-1247-1248-1249: August 2016 Monthly Sample

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-1247-1248-1249), pulled on 08/22/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-1247-1248-1249 indicated the Isopar™L concentration is above its nominal level (101%). The extractant (MaxCalix) and the modifier (CS-7SB) are 7% and 9 % below their nominal concentrations. The suppressor (TiDG) is 63% below its nominal concentration. This analysis confirms the solvent may require the addition of TiDG, and possibly of modifier and MaxCalix to restore then to nominal levels. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended. At the time of writing this report, A solvent trim batch containing TiDG, modifier and MaxCalix, was added to the SHT (October 2016) and expect the concentration of these components to be at their nominal values.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Characterization of infrequent samples from the concentration, storage and transfer facility: leak detection box (LDB) drain cell sample LIMS# 20195

Savannah River Remediation Engineering (SRR-E) requested that the Savannah River National Laboratory (SRNL) analyze the Concentration, Storage, and Transfer Facility (CSTF) samples from the following Tank Farm areas: the sump encasement, catch tank, drain cell and waste tank annulus. In general, these CSTF samples will be analyzed on an infrequent basis and analyses will include detection for total beta/gamma, total alpha activities and pH measurements. This report presents characterization results for the Leak Detection Box Drain Cell (LDB-DC) sample. The results are measurements for total gamma, total alpha, total beta, pH, density, anions, elementals and total mercury for the LDB-DC sample.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Quantitative Mapping of Nanoscale Chemical Dynamics in Sub-sampled Operando (S)TEM Images Using Spatio-Temporal Analytics

One of the main limitations in the use of operando scanning transmission electron microscopes to study dynamic chemical processes is the effect of the electron beam on the kinetics of the reaction being observed. Here we demonstrate that a flexible Gaussian mixture model can be used to extract quantitative information directly from sub-sampled images, i.e.~images where not all the pixels in the image are illuminated with the beam. The use of this method is demonstrated for the charge/discharge cycle of a Li-battery, where the deposition and dissolution of Li at the anode can be accurately quantified for sub-sampling levels down to 1%. Performing operando imaging using a small fraction of the pixels means that the observations can significantly reduce the effect of the beam, automatically increase the imaging speed and decrease the total data transfer rate required. Such new software capabilities offer the potential to significantly widen the application of operando hardware approaches to study nanoscale dynamics in materials.

Stanfill, Bryan A.↗

Electrokinetic Sample Preconcentration and Hydrodynamic Sample Injection for Microchip Electrophoresis Using a Pneumatic Microvalve

A microfluidic platform was developed to perform online electrokinetic sample preconcentration and rapid hydrodynamic sample injection for electrophoresis using a single microvalve. The PDMS microchip consists of a separation channel, a side channel for sample introduction, and a control channel which is used as a pneumatic microvalve aligned at the intersection of the two flow channels. The closed microvalve, created by multilayer soft lithography, can serve as a preconcentrator under an applied electric potential, enabling current to pass through while blocking bulk flow. Once analytes are concentrated, the valve is briefly opened and the stacked sample is pressure injected into the separation channel for electrophoretic separation. Fluorescently labeled peptides were enriched by a factor of ~450 in 230 s. The performance of the platform was validated by the online preconcentration, injection and electrophoretic separation of fluorescently labeled peptides. This method enables both rapid analyte concentration and controlled injection volume for high sensitivity, high resolution capillary electrophoresis.

capillary↗

Determining aromatic and aliphatic carboxylic acids in biomass-derived oil samples using 2,4-dinitrophenylhydrazine and liquid chromatography-electrospray injection-mass spectrometry/mass spectrometry

Converting biomass to a useful fuel commonly incorporates the pyrolysis of the biomass feed stock. The base liquid fraction usually contains high concentrations of ketones, aldehydes and carboxylic acids, of which each can cause detrimental issues related to the storage and upgrading process. Knowing the carbonyl species and the concentration of each will provide value information to the pyrolysis researchers, specifically as that community branches into more targeted end-products such as jet fuel or biogenic-derived oxygenate-containing fuel products. The analysis of aldehydes, ketones and small alkyl carboxylic acids using 2,4-dinitrophenylhydrazine (DNPH) derivation method has been well documented and the method is commonly used the analytical community. By using liquid chromatograph coupled to tandem mass spectrometry, biomass sample analysis can be complete with identification of most carbonyl species. The issue of identifying isobaric ketone and aldehyde compounds can be resolved by utilizing differences in retention time or characteristic fragment ions of ketones and aldehydes. One issue which could not resolved using published methods was identifying aromatic or large non-aromatic carboxylic acids from their corresponding hydroxyl aldehyde or ketone analogs. By modifying the current method for determining carbonyls in biomass samples, carboxylic and hydroxyl-carbonyl can be determined. A careful adjustment of the pH during the extraction procedure and extended heating time of the DNPH solution allowed for the successful derivation of aromatic carboxylic acids. Like other dinitrophenylhydrazones, carboxylic acid derivatives also produce a unique secondary ion pattern, which was useful to distinguish these species from the non-acid analogs.

bio-oil↗

An Open-Cell Environmental Transmission Electron Microscopy Technique for In Situ Characterization of Samples in Aqueous Liquid Solutions

The desire to image specimens in liquids has led to the development of open-cell and closed-cell techniques in transmission electron microscopy (TEM). The closed-cell approach is currently more common in TEM and has yielded new insights into a number of biological and materials processes in liquid environments. The open-cell approach, which requires an environmental TEM (ETEM), is technically challenging but may be advantageous in certain circumstances due to fewer restrictions on specimen and detector geometry. Here, we demonstrate a novel approach to open-cell liquid TEM, in which we use salt particles to facilitate the in situ formation of droplets of aqueous solution that envelope specimen particles coloaded with the salt. This is achieved by controlling sample temperature between 1 and 10°C and introducing water vapor to the ETEM chamber above the critical pressure for the formation of liquid water on the salt particles. Our use of in situ hydration enables specimens to be loaded into a microscope in a dry state using standard 3 mm TEM grids, allowing specimens to be prepared using trivial sample preparation techniques. Furthermore, our future aim will be to combine this technique with an in situ light source to study photocorrosion in aqueous environments.

47 OTHER INSTRUMENTATION↗

Validation of selection function, sample contamination and mass calibration in galaxy cluster samples

ABSTRACT We construct and validate the selection function of the MARD-Y3 galaxy cluster sample. This sample was selected through optical follow-up of the 2nd ROSAT faint source catalogue with Dark Energy Survey year 3 data. The selection function is modelled by combining an empirically constructed X-ray selection function with an incompleteness model for the optical follow-up. We validate the joint selection function by testing the consistency of the constraints on the X-ray flux–mass and richness–mass scaling relation parameters derived from different sources of mass information: (1) cross-calibration using South Pole Telescope Sunyaev-Zel'dovich (SPT-SZ) clusters, (2) calibration using number counts in X-ray, in optical and in both X-ray and optical while marginalizing over cosmological parameters, and (3) other published analyses. We find that the constraints on the scaling relation from the number counts and SPT-SZ cross-calibration agree, indicating that our modelling of the selection function is adequate. Furthermore, we apply a largely cosmology independent method to validate selection functions via the computation of the probability of finding each cluster in the SPT-SZ sample in the MARD-Y3 sample and vice versa. This test reveals no clear evidence for MARD-Y3 contamination, SPT-SZ incompleteness or outlier fraction. Finally, we discuss the prospects of the techniques presented here to limit systematic selection effects in future cluster cosmological studies.

79 ASTRONOMY AND ASTROPHYSICS↗

Dark Energy Survey Year 3 results: calibration of lens sample redshift distributions using clustering redshifts with BOSS/eBOSS

ABSTRACT We present clustering redshift measurements for Dark Energy Survey (DES) lens sample galaxies used in weak gravitational lensing and galaxy clustering studies. To perform these measurements, we cross-correlate with spectroscopic galaxies from the Baryon Acoustic Oscillation Survey (BOSS) and its extension, eBOSS. We validate our methodology in simulations, including a new technique to calibrate systematic errors that result from the galaxy clustering bias, and we find that our method is generally unbiased in calibrating the mean redshift. We apply our method to the data, and estimate the redshift distribution for 11 different photometrically selected bins. We find general agreement between clustering redshift and photometric redshift estimates, with differences on the inferred mean redshift found to be below |Δz| = 0.01 in most of the bins. We also test a method to calibrate a width parameter for redshift distributions, which we found necessary to use for some of our samples. Our typical uncertainties on the mean redshift ranged from 0.003 to 0.008, while our uncertainties on the width ranged from 4 to 9 per cent. We discuss how these results calibrate the photometric redshift distributions used in companion papers for DES Year 3 results.

79 ASTRONOMY AND ASTROPHYSICS↗

Sample variance in the local measurements of the Hubble constant

The current >3σ tension between the Hubble constant H 0 measured from local distance indicators and from cosmic microwave background is one of the most highly debated issues in cosmology, as it possibly indicates new physics or unknown systematics. In this work, we explore whether this tension can be alleviated by the sample variance in the local measurements, which use a small fraction of the Hubble volume. We use a large-volume cosmological N-body simulation to model the local measurements and to quantify the variance due to local density fluctuations and sample selection. We explicitly take into account the inhomogeneous spatial distribution of type Ia supernovae. Despite the faithful modelling of the observations, our results confirm previous findings that sample variance in the local Hubble constant ($H$ $^{loc}_{0}$) measurements is small; we find σ ($H$ $^{loc}_{0}$)=0.31km s -1 Mpc -1 a nearly negligible fraction of the ~6 km s -1 Mpc -1 necessary to explain the difference between the local and global H 0 measurements. While the H 0 tension could in principle be explained by our local neighbourhood being a underdense region of radius ~150 Mpc, the extreme required underdensity of such a void (δ ≃ -0.8) makes it very unlikely in a ΛCDM universe, and it also violates existing observational constraints. Furthermore, sample variance in a ΛCDM universe cannot appreciably alleviate the tension in H 0 measurements even after taking into account the inhomogeneous selection of type Ia supernovae.

79 ASTRONOMY AND ASTROPHYSICS↗

Design and instrumentation for permanent magnet samples exposed to a radiation environment

This work is part of a larger program to study the effects of radiation on permanent magnets in an accelerator environment. In order to be sure that the permanent magnet samples are accurately placed, measured, and catalogued we have developed a system of sample racks, holders and measuring apparatuses. We have combined these holders and measurement racks with electronics to allow a single computer to catalogue the position and intensity of the magnet measurements. We outline the design of the apparatus, the collection software, and the methodology we will use to collect the data.

Accelerator Physics↗

Solvent hold tank sample results for MCU-14-943 and MCU-14-1061: November 2014 monthly samples

SRNL received two sets of SHT samples (MCU-14-943, pulled 11/28/2014 and MCU-14-1061, pulled on 12/03/2014) for analysis. The samples were combined and analyzed for composition. Analysis of the combined sample (MCU-14-943-1061) indicated low concentrations of the suppressor (TiDG) and modifier (CS-7SB) despite the addition of TiDG to the solvent in October 26, 2014. However, the TiDG level in this sample is within recommended operating parameters. The solvent’s density is at nominal value despite the low modifier level. No impurities were observed in the solvent at this time. The laboratory will continue to monitor the quality of the solvent in particular for any new impurity or degradation of the solvent components.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Solvent Hold Tank Sample Results for MCU-15-389-390 and MCU-15-439-440-441. February 2015 Monthly Samples

Savannah River National Laboratory (SRNL) received two sets of Solvent Hold Tank (SHT) samples (MCU-15-389 and MCU-15-390 pulled on February 23, 2015 and MCU-15-439, MCU-15-440, and MCU-15-441 pulled on February 28, 2015) for analysis. The samples in each set were combined and analyzed for composition. Analysis of the composite samples MCU-15-389-390 and MCU-15-439-440- 441 indicated a low concentration (~ 92 to 93 % of nominal) of the suppressor (TiDG) and slightly below nominal concentrations of the extractant (MaxCalix), but nominal levels of the modifier (CS-7SB) and of the Isopar™ L. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent on February 22, 2015. Despite that the values are below the target component levels, the current levels of TiDG and MaxCalix are sufficient for continuing operation without adding a trim at this time. No impurities above the 1000 ppm level were found in this solvent. However, the p-nut vials that delivered the samples contained small (1 mm) droplets of oxidized modifier and amides. The laboratory will continue to monitor the quality of the solvent in particular for any new impurity or degradation of the solvent components.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Sample Results from Routine Salt Batch 7 Samples

Strip Effluent Hold Tank (SEHT) and Decontaminated Salt Solution Hold Tank (DSSHT) samples from several of the “microbatches” of Integrated Salt Disposition Project (ISDP) Salt Batch (“Macrobatch”) 7B have been analyzed for 238 Pu, 90 Sr, 137 Cs, Inductively Coupled Plasma Emission Spectroscopy (ICPES), and Ion Chromatography Anions (IC-A). The results from the current microbatch samples are similar to those from earlier samples from this and previous macrobatches. The Actinide Removal Process (ARP) and the Modular Caustic-Side Solvent Extraction Unit (MCU) continue to show more than adequate Pu and Sr removal, and there is a distinct positive trend in Cs removal, due to the use of the Next Generation Solvent (NGS). The Savannah River National Laboratory (SRNL) notes that historically, most measured Concentration Factor (CF) values during salt processing have been in the 12-14 range. However, recent processing gives CF values closer to 11. This observation does not indicate that the solvent performance is suffering, as the Decontamination Factor (DF) has still maintained consistently high values. Nevertheless, SRNL will continue to monitor for indications of process upsets. The bulk chemistry of the DSSHT and SEHT samples do not show any signs of unusual behavior.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Sample Results From Routine Salt Batch 7 Samples

Strip Effluent Hold Tank (SEHT) and Decontaminated Salt Solution Hold Tank (DSSHT) samples from several of the “microbatches” of Integrated Salt Disposition Project (ISDP) Salt Batch (“Macrobatch”) 7B have been analyzed for 238 Pu, 90 Sr, 137 Cs, cations (Inductively Coupled Plasma Emission Spectroscopy - ICPES), and anions (Ion Chromatography Anions - IC-A). The analytical results from the current microbatch samples are similar to those from previous macrobatch samples. The Actinide Removal Process (ARP) and the Modular Caustic-Side Solvent Extraction Unit (MCU) continue to show more than adequate Pu and Sr removal, and there is a distinct positive trend in Cs removal (increasing cesium decontamination), due to the use of the Next Generation Solvent (NGS). The bulk chemistry of the DSSHT and SEHT samples do not show any signs of unusual behavior.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Solvent Hold Tank Sample Results for MCU-16-270-271-272: February 2016 Monthly Sample

Savannah River National Lab (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-270-271-272), pulled on 02/21/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-270-271-272 indicated the Isopar TM L concentration is above its nominal level (101%). The modifier (CS-7SB), the extractant (MaxCalix), and the TiDG concentrations are 7%, 6%, and 40% below their nominal concentrations. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent in November 2015. Based on the current monthly sample, the levels of TiDG, Isopar TM L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Solvent hold tank sample results for MCU-16-1363-1365. November 2016 monthly sample

Savannah River National Laboratory (SRNL) received one set of three Solvent Hold Tank (SHT) samples (MCU-16-1363-1364-1365), pulled on 11/15/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-1363-1364-1365 indicated the Isopar™L concentration is at its nominal level (100%). The extractant (MaxCalix) and the modifier (CS- 7SB) are 8% and 2 % below their nominal concentrations. The suppressor (TiDG) is 7% below its nominal concentration. This analysis confirms the trim and Isopar™ additions to the solvent in November. This analysis also indicates the solvent did not require further additions. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗