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Abstract  

Analytical procedures for measuring various radionuclides in the238U and232Th chains in briney waters are described. Using methods such as mass spectrometry, and alpha, beta and gamma spectrometry, the desired measurement sensitivity required for each of the radionuclides is achieved.233U,228Th,208Po,212Pb, and133Ba are used as tracers for chemical yield recoveries. Typical precision of the results range from 5–20%.

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Summary

Galantamine hydrobromide was subjected to oxidative stress degradation using hydrogen peroxide and analyzed as per the chromatographic conditions described in European Pharmacopoeia. The drug showed considerable degradation at ambient temperature resulting in the formation of two degradation products at relative retention times (RRTs) 0.63 and 2.52. The minor degradant at RRT 0.63 was identified as galantamine N-oxide. The principal degradant formed at RRT 2.52 was found to be unknown and has not been reported previously. The unknown impurity was identified by liquid chromatography-tandem mass spectrometry (LC-MS/MS) followed by isolation using semi-preparative high-performance liquid chromatography (HPLC). The isolated impurity was characterized using one-dimensional, two-dimensional nuclear magnetic resonance spectroscopy (1D and 2D NMR) and elemental analysis (EA). The principal degradant was found to be formed due to the generation of bromine and subsequent attack on the aromatic ring via in situ reaction between hydrogen bromide and hydrogen peroxide. The unknown impurity was characterized as (4aS,6R,8aS)-5,6,9,10,11,12-hexahydro-1-bromo-3-methoxy-11-methyl-4aH-[1]benzofuro [3a,3,2-ef] [2] benzazepin-6-ol.

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Abstract  

NiMoO4 obtained by calcination of precursors has been shown to be a very effective catalyst for oxidative dehydrogenation of propane into propene. Preparation conditions and thermal decomposition of two precursors have been studied by TG-DTA, HTXRD, FFT-IR, and thermo-desorption coupled to mass spectroscopy in order to determine their composition and to define the best treatment to favour the oxidative dehydrogenation process. The selectivity and activity for propane transformation into propene are very different depending on the nature of the precursor and of the active phases obtained after thermal activation. The more selective high-temperature β phase of NiMoO4 has been obtained at a lower temperature (500°C) than previously reported (700°C).

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Abstract  

Three different spent control rods were obtained for direct-assay measurements and empirical sampling and analysis. They were: 1) a BWR cruciform control rod, 2) a PWR rod-cluster control assembly, and 3) a burnable poison-rod assembly. The dominant activity of the BWR cruciform control rod and the PWR burnable poison-rod assembly is60Co, whereas the PWR rod-cluster control assembly is dominated not only by60Co, but also by108mAg and110mAg, which are found in the Ag–In–Cd alloy of the absorber rods. The radionuclide inventories calculated for the three spent control rods from the empirical sampling data agree very well with data determined from the two direct assay methodologies. The concentration of108mAg in the rod-cluster control assembly will have to be considered when these types of spent control rods are prepared for waste disposal.

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Abstract  

Fluorine surface contamination and depth profiles were studied using the19F(p, p')19F resonance reaction. Fluorine implanted silicon samples as well as ZrNb plates and Cr–Al layers after a HF-treatment have been examined. The resonance strengths of the narrow 1088 keV resonance were estimated.

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Abstract  

Hydrogen surface contamination and depth profiles can be measured by the resonant nuclear reactions1H(19F, )16O and1H(15N, )12C. The method was applied to study hydrogen-implanted silicon, amorphous silicon layers and silicon oxide films produced by anodic oxidation.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
D. Robertson
,
V. Thomas
,
H. Rieck
,
D. Haggard
,
W. Reece
,
J. Pappin
,
W. Hensley
,
D. Brown
,
C. Thomas
, and
P. Robinson

Abstract  

Battelle, Pacific Northwest Laboratories has recently developed, tested and field-demonstrated a technology for the direct assay of transuranic radionuclides (TRU), fission products, and activation products in a variety of radwaste packages generated at commercial nuclear power plants. This technology involves non-destructive passive neutron counting for determination of nanocurie/gram quantities of the TRU radionuclides. Direct gamma spectrometry combined with thermoluminescent dosimetry (TLD) and correlation analysis is also utilized to determine the concentrations of the fission and activation products present in the radwaste packages. Employing counting times of 10 to 20 minutes, a complete analysis of all radionuclides specified for assay by the U.S. Nuclear Regulatory Commission (in 10CFR61) prior to shallow-land disposal of commercial radwastes can be measured at concentrations at least tenfold below the least restrictive Class A waste catagory.

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Abstract  

The Comprehensive Test Ban Treaty calls for the monitoring of aerosol radionuclides throughout the globe. Pacific Northwest National Laboratory has developed the Radionuclide Aerosol Sampler/Analyzer (RASA) for the Department of Energy to automatically collect and measure radioactive aerosols from the atmosphere. The RASA passes high volumes of air through a 3MTM Substrate Blown Microfiber Media (SBMF) specifically designated as SBMF-40VF. It then automatically moves the filter media in front of a high-purity germanium detector and collects a gamma spectrum. If further analysis on the filter is desired, the filter is sent to a laboratory and radiochemical analysis is performed. This paper discusses the method of dissolution of the SBMF-40VF filter media and the separation of the radioisotopes of interest.

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Abstract  

A review is presented summarizing the specific nuclear microanalysis methods applied in our laboratory to study amorphous semiconductor thin films. For backscattering, ∼3 MeV Li ions are applicable when depth resolution and sensitivity are required while up to 8 MeV α-particles allow larger depths to be probed and elemental interferences to be solved. These features are predominant for diffusion studies between metal electrodes and chalcogenide films. On the other hand hydrogen profiling using the1H(1 5N, αψ) resonant nuclear reactions is described and analytical problems associated with its use are discussed. Applications to the elaboration conditions of hydrogenated (a)Si is developed.

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Abstract

The Madaras brickyard section found at the northernmost fringe of the Backa loess plateau is one of the thickest and best-developed last glacial loess sequences of Central Europe. In the present work high-resolution magnetic susceptibility measurements (at 2 cm) were implemented on samples from the 10 m-section corresponding to a period between 29 and 11 KY cal b2K. One aim was to compare the findings with the ice core records of northern Greenland in order to establish a high-resolution paleoclimatic record for the last climatic cycle and with findings documented in other biotic and abiotic proxies so far. Our results revealed a strong variability of loess/paleosol formation during MIS 2. Millennial time-scale climatic events that characterize the North Atlantic during the last climatic cycle have been identified. From 29 ka up to the start of the LGM, the recorded MS values show a weak, negative correlation with the temperature proxy, and a weak positive correlation with the dust concentration of Greenland. A strong correlation was observed with the local paleotemperatures. Local climatic factors must have had a more prominent effect here on loess/paleosol development than the climate shifts over Greenland. During the LGM the same pattern is seen with a stronger correlation with the dust concentrations and a weaker correlation with the local temperature. Local climatic factors, plus dust accumulation, must have had a prominent influence on loess/paleosol development here. From the terminal part of the LGM a strong positive correlation of the MS values with the temperature proxy for Greenland accompanied by a strong negative correlation with the dust concentration values is observed. Correlation with local paleotemperatures is positive and moderate, strong. Here climate shifts over Greenland, as well as local endowments equally had an important role on the development of the MS signal.

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